CIA Preparacion Explosivos

F~e]d Expedient Metbods: fOir Explosives Preparations

@. 1:vn by Desert PubiLicatiolils P.o. Bo,>;: rrsr

11:1 J)or.m<l, AR 7.'3h1751 !!JOI1·862·2Mi

mS.HN 1)..:s7941·2M"J I§: 14 113 U 11 ]:0Ji PrinMJed :i!!! U. S. A.

Dese.ft I\IblJJC1ltiotl Is a dMsiOill. of The DEL TA GROUP Hid,

DiJJfd al.11 iliUllWJFeS & ,orden; ~o' (h,e .lliIXllIie address,

All rigbJIS reserved, E.tC~t roc use in a re v ew, no, portion ofdlis ·book m ~y be reproducoo by any means knw'n or unklilOiwflI wiUl(l1Jt the: express wriuen perrnlssion of lhe pIiMishe:r.

Neither tilt: autnor nor ine pulblishcr 3S11UIf es ll11.y re!ip9I1i>ibili Iy for the use' or mi~lIse. crf the: j];f(jnn:ll[:io~ centamed in fu-ls oook.

TABLE .oF CONTENTS

SE-'TION I

,Fi!tld ExpedieJlt Metil .. eds

for Ex.PJloslvee Prepl{W!;tion., _ , " •.• , • , •••• , , " • •• .• 1

Preparation of Lead P:i~FaiOO'. , _ . _ ., __ , • , • , _ .' • " •••• _ 1 Preparstio.!l: or Picric AeidlJh:o'm ~prm , _ . _, __ . < , " , a 1'etf.:ammineco:p[iXlr ([I)I ChIQntw , _ , __ e •• , • , • , • " •• _ 6 Potmsium (or Sodium) Nitriw

and Lithw:rge ('Lead Monoxide) _ ••••. , • , _ " _ ...•.•• 9'

P:re,p.a:mtiml of Co'ppe:1" SulfatE! (P<3ntah~'d!~~}. , • " _ .. _ 12 R~cB~lDatJ..ol1 0"1 RDX FTom C-4.,' ... " , _ .. _, _ , . , ...• 14

8:iECTJON ]I l4Il;mmtory Mo::tbod!i

for P.lieparillg.l'[lotl'lli:!itlilill E,,;:plosivGS . __ ,,- , •••.••• " _ ' •• '. 17

Leacl ... '\;zidi;!' , , •.• ,. " . _ " _ .••... , • , • , " , • _ , • , •• " ,,' 17 Niw~ureOll" _ • , • , • , • , •• " " .. _ . _ . , , , , •..• , ... __ .. _ 20

M~nnitoU HexMlim.te ~filwmaJij.J1itJrol . , _ .. _ , , , . _ • , • 21

Ch1oRoommeru.D:!I'Cetaidetlyde ••••••. , • , . _ .. " 22

Trts.l!'iytlr..a:idnez.inc (U) Nltrare . , . , , , .. ' . , . , , . _ ,. ::;:,3

F'mmi.llatiing Sll\lel', , , .. _ .. _ ... _ .. , . , .• , . " , __ , .. " 23 D]l!Ilt'J.mi:r!l~5ij.'e<r (1) Chlorate • , • " , " • , __ • , .• , • • • •• 24 Triacetol'letripC!.I'oxidli , , , . , ...• _ ,. ,. , , • , •.• , •. _,,, 24

....

ilii

FIELD EXPEDIENT lVIETHODS FOR

EXPLOSIVES PREPARATION

PREPA'RAT[ON OFL<EAD P1CRATE

Lead Picra:te is usecss a. primary explosive, in the b..br'1C<'IItioru of tieton,atoI"s. It 'is to be used witha boO~S[I;T explostve such asptcrtc acid or RDX"

Litharge (lead monoxide), {field prepa:h"ed; a] ffi 0' i@ used 1itlL plum,bing and ceramic CBmel1lts),

P tcrlc ac id (field prepared)

Wood.dcohol (metharlol) . ~:sottJ.e antifr'eezes and palntremevere]

Wood!ell or plastic Fod

Improvised scale ~see seettcn VH. No.8)

11

P'ROCEDURE~

1. Weigh out 2 grntns (orequu] amounts) by weight O'f picric acid and lead monoxtde,

2. A.cld the picric acid to ~ teaspoons (10 ]1].iUUiters) Ofl1flBfu!mO:~ in a container (dish 01' sa ucer) and stir.

4. Continue f'iti:rring and allow the' alcohol to ,evaporate., NOTE;' Themtxture will suddenly llit cken,

~. Carefully b'J:'ieak up this m~xtureatid sttr occasionally untili a: povilder ts formed (21 f,ew .~UInp'S will remain).

6. Remove B.J]1d spread ~)U:t eo air dry. NOTE:: [f posslble~ d:ry at, 100°C (212 F)

lio:!' two hours. -

PREPARATION OF P[CRiC ACID FROM ASPIRrrN

picric aetd C!1In be used 8[,3 a booster explosive hI detonatQl'S or as an tntermedtate to prepartng lean pi.'craute or DDNP,.

Aspitiu.~ 20 taMets (5 grahlltab~et) A.rucohol ~ 95 pereent pUre

C{).ocentr~ted suUu:ric acid (hoH batteI'll acid until wMte fume~a:ppear)

Potaasi um urtr f)j~. ts all tpeterj Water

Hot water bath

.Pa.P6[, towels (for fnter)

Glass tube or rood!

Di s h ((:~ramic orr glas s)

3

Cup

PROCEDURE:

I. Crush 20 tablletso[ aspirin in a glass '(:CII1:t~ine:r. and work ~nto a paste wtth a: teaspoon of water.

2.. ~~d appI'oxtma.tely 1/3 " JIl/ 2; cup (1(10 m]lhhte'l's) of alcohol with stirring and filter through a paper towel into another gl aas COI![catner.

If asptrtn is pure enough (usually cheap pr'iced aspirin are) then Ste1Js I, .2 and 3 can he omitted and. can proceed and add crushed asptrtn w S.ulfuric .Actd.

. 3. Discard the. sohd left en the paper' and pour the Iiquid from the container into the di sh, .Evapor ate tbearooncl and W'Mer On a hot water bath, leaving: a white powder,

4 -. _ Add this white powder to 1/3 cup {SO mfUil ite.l;"s} of concentr-ated sulfurto acid in a. canning j 8.L]" .•

5. Heat the- jar in a simmering hot water bath far 15 minutes and remove. Stir; solut~OJ] wUl g:raduaJIly tuTn bbu::k.

4

,6:. ~dd 3~ le veJ . teaspoons (15 gl," am 13) of potaasium nttr-ate In three portions with vigor- . o us stirring, After he.at;i ng put j [ll' in cold H .20 and acid KNO .3.

7... AUow the yeHo·w-or aJilge solution to cool to roorn temper-ature with intermittent s.tir~ ri.ng, Solution lE; darker than yenow-orange.

8. Pour the s,oluUon into 1- 1/4 cups (300 millHiters) . of water [cold if posstblej and allow to cool, Upon pouring. soluttcn 15 now

y@llow-oraJllge. .

9 .. Filter the mix-tun! through a papertowel and wash the light yellow material (picric .amd) wtth ]! SCUll' (25 milliliters) of water through paper towel. Takes cons i der able time to fUter if gennine filter paper is used .

J.O. Dry at 160-.200 °1' for tWfJ hours. The yield ii84.0 - 4.!;i grams.

5

TETHAM1l1JN'ECOPPER UI} CHLORATE

Tetramm tnecoppe r (1Q chlorate is a prfmary explo,stve that Call be made fr-om sodium chlorate. copper iSUl.fate~ and ammenta, Thls explcstve when used wtth a booster- ts eapable of d,etQ~'la!tjtl.g compoettlon C-4.

11,.'IfATEmAL REQUl.RED:

Sodium cblcrate (obtatn as medicine, weed kiner. deiolhmtt or by field method)

'Coppelr sulfate (o,'otain !i1,8 tns·ecUcf(ie. water pUl'Uytng agent, 01' by fie~dI method)

AW1l1! onium hydro.xJ d@ (O bta in as .bousaoo'l d ammonia OJ' Blnentng salts)

Wax or clay

\V.abe·r

N an-ow mouth bottle (wine or coke)

W1de mouth bettles (mason jill's)

'I'ublng (rubbel"., copper, steel)

Im Pl"O,V 1 se d seaue (see sectten V n , No.8)

Heat source

Paper towel (foJ" inter),

Pan

PROCEDURE:

1. Me esure ]. /oS teaspoon {2. 5 grams) of sodtum chlorate in a wide mouth bottle. then add ]lO teaspecns of alcohol.

2. Add 1 teaspoon (4: grams) of copper" sulfa,tre and stir. the mixture JIU8t under the boHing point fot 30 minutes (heat can. ~e suppli~~ by a :pan of hoe watJe:r)., The mlXhtFe wlll change color. NOTE; Keep solut ion away from flame,

3, Keep votume of the solution. constanfby adding additional alcohol about @v8r-y 10 mtnutes. Remove soluttoa and let coot Filter through folded paper 'towel s into another wide mouth bottle, Keep the 1 iquid ..

4. Add 1 Cl!1pr (250 mmmte['s) of ammonia to the narrow mouth bottle, Plactng tubing so ~hat ]textends about 1-112 inches hlsidebotUe~ then seal tubing: to bottle with W8IX (pttcn •. 01 aly • etc.).

"1

S. Pbce tubing into solution from step (B;) as indicated in the flgure (next :page).. He at bottle c~'Iltainlngarrn:J:rIo!lta tn a P.M of bat w:;tlter {not boiHng) fnr about U) rnhru'ves.

6., BubbTh.~ ammonta gas through solution until the, cO:W,ol' ·of the 00 ]1;]t iJOJ'J! changes from a Ugbtgreen to a daJrK blue {a.PPl"oxirnately 10 minutes) and continue bubbUng~for anQUIBl' ten mtnutes,

CAUTlON; At this potn; the so.li·ution is

0. Oil primary explosive. Keep away from flame.

f .. Redllt::e ilie vohm:moo the sol ut ion rOO about ]! 3 of its or igimal vot urne by eVOiJ)}j0rating in the ~tl," (1)1' h~ a streem of alr ..

8.Fntercrys,ta~s Uu:·ough. a foLded paper tow€l and wasbcnce w]tn 1. te aspcon flI]:cottoli. dry Qv'erni ght (16 hours).

r\ CAUnON: Explostve ts shock OO'id fhunc Iv senaitive, Store tn a: cupped container',

POTASSIUM (OR SODrUI'J.II) NITRITE AND LrrHARGE (LEAD MO~OXlnE)

Either of the nttrttes are needed to prepare DDNl? and litharge is required for the prep<ll'S)tion ()f lead ptcrate,

~1:ATEmAL REQUIRED~

Le ad metal (smaU pieces or oh 1]lS)

Wood (methyl) a:!lmhol

Iron pipe wU11 dosed ,end Or' Gap ~oneend only}

Iron :rod (scre\vdriver)

Paper towels

Gla.ss jar's, wide mO!j"th (.2 IB aen)

Pan (metal)

H.eartsouroe (sUich as hot coals or blow torch)

~-,

]mpl'ovisl3d scale ,(see' Section VU, No. S}

Cup

PROCEDURE:

L Mix :112 grams af lead and 4lP'ruJrlJ,g of potassium, (or sodium) nU:r<ite. Place [Jhe mmtu:re in the iron. contatner (tron pipe)1 and heat in a hot bed of coals or twa blow torch foil:' hour or mor-e,

2" RemOlve the contatner and allow to (lOO],. Chip out the y,~now soltd with the screwdr]ve~ and add to 1/2 cup ,(120 mmmters) of methyl ,a:J::coho] in ~he ] ar. Orange- Brown soUd" cream color tn alcohol,

~:,. He-at the mixture in a pari of hot waite r until i~ reacts. SohrtiOl1l~U:t[[![3 darker' upon, heating,

4. JFiUer the m'ilxtm:-e ~,]:U',Ciug:h a paper towel into th13 second j ar,

5., Th@ salid le:tft on the paper ls lead monoxide. Wa:sh tt (ltrough paper twice, using 1/ Z cu.p (120 milUUters) hot water ,each ttme and aliI dry before using tn e::!q)~Q:stve preparation (for' example, lead pin ate) .'

6. Place the jar with the liquid tn the hot water and heat U!ltU a], coh6J. has evaporate d .. The remoa iinin;g powder l s the nitrite, snowy liquid.; some wh tee powder appe arsbut not much,

NOTE: Sodtum nitrtte has a ~tton;gtendencjr to absorb wa~e:r from the atmosphere and should be st..oredi[1J. a closed container.

PREFARAT[QN OF COPPER SUL.f'AT.E (PENTAHYDRATE)

Copper sulf ate h:: a l"eq)u i red mater] al forl:he preparatton of T AC~ -

MATE RiAL REQUIRED;

Potas.stU!:ll ottrate or nitric aetd (Held gr'a.d~:s), Alcohol

Papel' towels

Metal pan (for hot water bath~

[mp1.'ovised scale (see Seotlon VI[" No.8)

Cup

12

PHOCEDUHE=

l.PlaoeWgrams of copper into one of the jarsand add one cup (24.0 mHlilttel's) of suifurtc (battery) acid, To this mixture add 12 gr ams cfpotas sdum nitrate. .0]' JI. .. ];2 te aspoons of nitrlc acid. NOTE: Nitric acrd gi yes a product of greater purity.

2. ileat the mixture on a hot w ater- b:;J!H~ (near boiling} until lli~ bubbling has ceased {re~ quires about two hours).

n CAUTION: Thisrea,citionevolves strong V toxic fumes and therefore must 1:Ie performed in an open; well ventilated ::tl.'!%I!.

;3: POiJt' the hot blue Iiquid into a second vessel (ke~ping the uureacted copper in the first jar) and all.ow to cool at room temperature,

4. After the ,crystals have tormec, i(~arefuUy pour away tbe .liQ.uid and. hI:'e'a,k up the Cf'y~ stalls. Then add ] /2: cup (120 mmiHt~rs) of

alco.hol to the powden and sttr. .

6.. PoOUl" t;he so,luUon U:rro~gh the tnwel f'ilter and waah the softd' left on the Ajapsl' tb:ree times, ustng 1/2 cup {120 miillli1 iter) port.ions of the alcohol each time,

6,.

Allow the pro duct to :aj r dry f or two houra,

13

HEC.LAMA1.'TON OF RDX FROM C"'i

RDX can be used as a booster explosive for detonators or as a hi.gh explostve charge,

MATERIAL REQUIRED:

Gasoline

C-4

Paper 'towels

Teaspoon

P'ROCEDURE:

1. Place 1 teaspoon (1.0 gr ,ocms,) ,of 0·4, in thie ptnt jar and add one cup (2A0 mtlltl.iters) of gascltne,

2 .Kne ad and still' the (:-4 i'i' ]th the rod until the C--4 has broken up. AHow to stand 1/2 hour.

114

3. StM"t U'l.~ stlr-rtng agatn unttl a nne white powde r rem a ins on the bottom of the contamer.

4L F'ilter' the mtxtura through a pap-er towel and wash the sol id left OD the paper with I /2: cup (ill20 mHUliliers.) 'Of gasoline.

5,. Air dry for several hours or beat at 80~HlOo C (aboLlt ]50-212 of) for ant'! hour.

#

;.- .

15

LABORATORY METHODS FOR PREPARING

PROMISING EXPL08IVE8

Preparatuon of Hydrazintum SuU'afie.

2 NHS +- NaOCl + H2.S04~N2 :rr4,' H2S04 + N:aCl + H20

One-hundred-forty-one ml of Chlorax bleach (5.25 preceat NaOC1.} was acr;1~ed to .200 ml of .20 percer.w.t ammontcm hycl:r.o:xJde and 5mL of 1 percent Hnnewater Ca. (OH12 in a one litel!:' Erlel1!meyer fl~k. The mixtUlre was rapidly heated to boiling and maintained unltil the Vobd'neWaS ·:t:'edluic~d. to about hill, which required about on.e':half h(Hl'l'. The solution WO:l!8: I'S!!pidly 0ti6~li$d and dilute, suU!lric acid. was €J!.dded 1!tntH. a pH of 7-8 was attruhl.edand the prectpltate that formed was sepal'awd by filtration. Tht:.c.,:,ld filtr!il1te was strongly actdifted with 40 percent su]:~ fur~lc acid. The white precipitate was filtared, washed wtth methanol and Bl~T dr'i ed, MtdUng point 254 j:' 2°(; U[t. 254 0q ..

A mixh.ill"e of 45 ml concentr-ated sulfuric actd, 31) rnl water and, UO ml isopropyl arcohot, previously cooled to OO'Cj was add.ed to am tee cold scdutton of 114 grams of sodium nitr-ite in 450 ml of H. 20. SiO~f ,addi~ bon requrred about two hOUll"S, in o:rder to maintatn t'empel'a,tul"e around OoC. The upDe.r oUy lay,er was separ-ated and \VaShBd three times with ,30 ml portions of 5 gram 100 1111 sodium bicarbonate solution and 22 grama NaCl 1.00 ml solution respectively,

Preparatfon of Sodium Azide"

N :aU.!!:" HI 20 + NaOH + C.4He ONO 2 ,.....;;. NfJlN 3. + C 4H '9,OH + 3HJ 20

Fiv,e grams .of caustle soda (NaOMi) was dtssolvedin 5(1 !lli], of ethyl alcohol (,3A)o" and the cl.ear portion was decanted in a 100 ml distilling flask c'Ontaining 6m! of hy,draz, ine hydrate, Mt-er adding - one, ml of butyl nitrite (or isopr,opyl nitrite) the mixture was heated on a steam hath toi::!:Uiate tile reaoHOlD.. 'Twe·h7e ml mor-e of the nitrite was s~(lwly added in ~uch a manner that the mixture reflux,sd slowly. Arldit{(),n req,.uJred about one hour and the mbo;lure was heated an ~dd1tionaI fjfteen minutes. The reaction

l8

tlas.k was cooled and the solid product col .. Iected on a filter. The product was washed wtth alcohol and air dr ied, Becrystalltaa .. tion from water yielded. white crystalltne mntertal.

" Lead! A~ide_

The follow~ng soluttons WII;'I'e pre ..

paredi

Solution A: O.2tO g of sodium azide and 0.006 gofsodt.um hydoxi.tl!e in? m] of water ,

Sohrtion B~ 0.,6:9 gr<'il.m~ Pb (NOa) 2 and 0.04 grama Dextl'in di asolved in aSColuUQIl. 0'1 9 ml water. This soluUon i s bI'oOu;gtl.t to a pH oJ ,5 by t-he addttton of dilute N.aOH.

SO]1L!![ ion B was brought to 61P' C and Solution A was slowly added with sUr]"ing~ The mh:llture was allcwed to ettr Ull! ambient temperature was attained and the soud azide cullected on a fUt,e'l"" Mtem> washing wUh water and air drying the prodact weighed 0.4 grams.. 'fhis pr-odluct WM found eepable of inttietlng RDX when tncorpor ated into a. No • 6 blasting c ap.

NrTROVREA

Urian NUra:be.

Tw~n.ty'-jftv,e ml of concentr-ated n~h:"ic acid was added dropwise toan tee cold solu~ ! 10,n of 5.0 gr ams mea in 26 ml ,of water, The white pren ].pit ate was co] leeted in a Buehner funnel and washed, wiJhicie coldnitr1c acid. After drying at 1000 C fol' one hour. yield W<tS 9.2 grams, .

Nine (9.01) gI':!m1J.S of the above pI'oduct~ urea n itrate ~ wag added :pol'it~onw tse to 32: ml of ice cold (-3.0 C) concentrated sulfuric acid at such a rate that the temner sture did not exceed 60 C. 'Total time for addition was approxtmately one-half hour. aft®r which the mixture was poured! [In 75 grams w ice. The whUe pr€tc]pita,te W~l.5 fUtered, washed wlth tce -eotd water, just 8tJffie~,ent to cover it, and air dr i ed, M ater-i al ohba.i:ne(l!\lle t gt.,ed [).3 g1'<lims and melted, with decomposjtten at 1570al!,5S0 C (lilt. 158-1590 q.

MANtilH'OL HEXANITRI\TEl NIl'ROMAWNlTO L

Tan grams of mar.mitoli was added pcrttonwtse to 50 ml' of conoentnated mtrto a~:i.d keeptng tlle temYl,erature at 00 c .. One .. hundred ml of eoncentrated sulfuriC alCid was then tlicida!iJ. dropwts e m atnt atning temper ature around 0 (I C. The sluTil"Y was fHt€,]:'ed ,j\ washed with water and a dilute Nn 2C02 solution and water aga; n, unti] waahinga w'®re neutral. .Prociuct was air~tried and had a melting point orr 11~H1HJ,o C (H.t.n2~1l30q,

LEAD NURANI.LATE

C ltk~!r ani.l i

A slurry of 5,,0 W!l!ms of sati.cyUc acid and :LOCI' ml of co[tOGl1I.tt'l3!.tedliydrocbloric actd was beated to 8[1 (I C o'li.nC1 ~~ •. O grams of potaS!3,lI,lm chlor~te added iIi. port"ion,S (with ,eff!llIV'e scencet • Ana-do ~Uo.mu. 4100 rol of eoneentr-ated hydrOcil}ol'i,C add ami 5.0 grams petasstum ehlorase was idded and the mtxtuee allowed to heat Sit B 0-900 C for f [It] r hOUTS, After fUliering, wasbtng wtth water antI atr d:ry1ng. t-he yellow crystals melted at:L90-200 0 (; (sealed tubej, The yield was

1- _ ~ _. '. -"'"" I

i5.<i@ grams ..

'" In Ue::Id lise. the insolllMe. stu.rry whtch HClI.mrG the lOp of the: so ~,I(:!ti on. m ~.y be decanted er see ()ip~ ed off.

Sodium N~tranilate.

A mtxture of 5.0 gram"" of chlorantl and 200 nll of ethyl alcohol were beaced to bOning and treated wUh .a solution Qf 5.6 grams of sodium nitrite in 100 luI of ethyl ~dClOhol. The mixture washeated wr'th sfirring for- one~h:Alf hnur and allowed to cool. l'b!e'O-l'ange-gold crystallfne product WM.Co.]~ Ieeted on a (Hter. washed with ethyl alcohol and air drted, Y i sld was 1.85 grams,

Lead N'ural'lilate.

. .A solunon o! 1. Ogr ams of sodium

nitl'anHate in 1(10 mt of boLing was fUtered .and ~e. fnt~ate treated w tth 2.9 .grams of le,1,ld nitr ate in 10 ml nf water, The m"ix:bJ re _w~aB a.tiirred for one .. hadf hliJUT and ~he gold platelets colleceed on a filter andwtth water. After drying at SO'I) C for three hours the product weighed_ 1.23 grams. The pro'duct ignU,edwifh a loud report on llama contact.

CLHORATOTRIMERCURlA CETALD'EHYDE

A stream of acetylene ~fro:m calcium eSll'b1de} was led into a solution of '0.,3 gT.am ,i)! mercurto nibateand O. iL gram sodium chlorate in 20 ml Qf water, The soltd SUS~ p ension W8.a. tntt iaJJy whUeth€ln turned gTey upon further traaement with acetylene'. The

product was co 11 acted on a filter ~ washed with water and all' dried, Ignition temper" ature was ca. 1500 C as determined wtth a F l sher-J ohns mel Hog po int appal" atus.

TRISHYDRAZINEZINC (II) NlTRATE

To a. solutton of 5,.0 geams of' zinc nitrate in 25, rnl 'Of ethyl alcohol was added a solutkm, of I, '7 ml of 95 percent bydraztne in S ml of' alcohol. The p'l'ecipitate that tmmedlately formed was eolleeted on a filter and washed 'with -ethyl alcohol. Mtel' dr:lttng for g.,5 houes at 90° C the product weig;l1.ed 4.4,5 gram So •

FULl<l:INA'f[NG SILVEH

Stiver ehllor-ide (from atlvee nitrate and hydrocntorto acid} was treated with suf .. ficie.nt ammonium hydroxide to effect solut ion. Tht i'i! solutton was tre abed with potas-

:sturn hydroxtde pellets until effervesc,ence subsided. The black mixture was diluted with water and the dark so,]id. oollected 0111 a Filter, Attempts 100 remove the"'p:roduotfrom the wet lIilter .resulted in all exploston,

23

DlAMMINESILVER (~) C~IWRATE

A near saturated soOlu:~i Oil of 8 H V15:r chlorate' (fll."Om silver nttr-ate and sodium chlorate), in water was treated c1!l'opw]se,wUh concentrated smmontum hyd:roxi.d€l;. The dark product mildly defla:gr;:tA;ed :after tscla .. Hem by fiUr aHon.

TR,[ACETONET RIPER-OXIDE

A mtxh:rre of 5 ml oJ! acetone and 10 mlof 6: percent hydrogen pe rO';'i:1de was cooled to 0 0 C and treated dr,o:lw'isewi th ::I rnl of eoneentt-ated :suHUl'iC actd, The white prectpttate 'tb:liI!!t formed W:'l1S md.ra.cted with ether and the extract was wasbedthreeumes with cold watwet'. The 'ether was ,evapoJ'<lJted by a: st re am (.lit a: l~ arid the pl'Odill!c(me[ted at 9 0-95'0 C. (Ii 1.. 94- 95 0 C.j

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