Lourdes Patricia L.

Carreon December 8, 2011 Zaborah Eunice Bobadilla, Nerissa Unielle Quenga, Bernadette Toledo

I. Objectives
  To synthesize tert-butyl chloride from tert-butyl alcohol using HCl as the hydrogen halide To purify the synthesized tert-butyl chloride using simple distillation

II. Schematic Diagram of Procedure

place 10 mL tert-butyl alcohol and 20 mL cold conc HCl

swirl mixture gently (don't shake)

open stopcock every now and then

allow mixture to stand for 20 mins

separate layers (discard aqueous layer)

transfer organic layer into dry flask with small amt of solid NaHCO3

swirl gently and decant to another flask

dry collected filtrate with small amt of anhydrous CaCl2

decant into dry 25 mL roud bottom flask

+ few boiling chips and distill crude tert-butyl chloride

collect pure tertbutyl chloride into 10 mL graduated cylinder cooled in ice bath

collect faction that boils at 49-52°C

submit product in labeled vial to instructor

Preparing a Simple Distillation Apparatus

prepare simple distillation setup

choose round bottom flask where sample fills 1/2 to 2/3 of its volume

place sample + 2-3 pieces of boiling chips or boiling sticks into flask

turn water supply on and check water flow through condenser

slowly heat sample in flask to a gentle boil

record boiling point

adjust flame so that distillation occurs at a rate of 2 drops distillate per second

discard first 1 mL of distillate and collect faction that distills at constant temp (boiling pt of volatile component)

remove heat source when sample starts to boil

allow entire set-up to cool before dismantling it

III. Table of Reagents/Products
Reagent/Produ ct Structure Physical Properties Hazards
Hazardous in case of skin contact (irritant, permeator) , of eye contact (irritant), of ingestion, of inhalation. Extremely corrosive. Inhalation of vapour can cause serious injury. Ingestion may be fatal. Liquid can cause severe damage to skin and eyes. Slightly hazardous in case of skin contact (irritant), of eye contact (irritant), of ingestion, of inhalation.

Tert-butyl alcohol



IV. Waste Disposal
  Aqueous solutions – dilute and pour into sink Organic compounds – proper waste jars

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