1H NMR (400 MHz, CDCl3) δ 4.82 – 4.71 (1H, br. s, NH), 4.67 (2H, s, H-11), 3.57 (2H, d, J = 5.

8 Hz, H-9),
2.21 (2H, m, H-2 and ), 2.19 (3H, s, H-13), 2.06 – 1.94 (2H, m, H-6A), 1.86 (2H, m, H-7), 1.76 – 1.60 (9H, m,
H-2, H-3 and H-6B);

C NMR (101 MHz, CDCl3) δ 213.2 (C, C-1), 154.8 (C, C-10), 95.6 (C, C-12), 74.7 (CH2, C-11), 57.3 (C, C-8),
13

43.7 (CH2, C-9), 38.0 (CH2, C-6), 35.0 (CH2, C-3), 32.5 (CH2, C-5), 30.4 (CH, C-2), 27.5 (CH, C-7), 26.9 (CH,
C-4), 24.9 (CH3, C-13).

2,2,2-trichloroethyl ((2-phenyl-1-oxaspiro[2.3]hexan-2-yl)methyl)carbamate (XX): Prepared using a

modification of general procedure XX (no 1 M HCl solution stir) using 4-phenylpent-4-en-1-ol (65.0
mg, 400 µmol), 2,2,2-trichloroethyl {[4-(trifluoromethyl)benzoyl]oxy}carbamate (183 mg, 480 μmol),
[Ir(ppy)3] (2.7 mg, 4.00 μmol, 1 mol%) and acetonitrile (2 mL). Purification by flash column
chromatography (SiO2, cyclohexane:diethyl ether – 9:1) gave the title compound XX (102 mg, 289
μmol, 72%) as a colourless oil;
1
H NMR (500 MHz, CDCl3) δ 7.38 – 7.32 (m, 2H), 7.31 – 7.27 (m, 2H), 5.08 (s, 1H), 4.70 – 4.66 (m, 1H), 4.21 –
4.12 (m, 1H), 3.47 (dd, J = 14.4, 5.1 Hz, 1H), 2.59 – 2.46 (m, 2H), 2.35 – 2.25 (m, 1H), 1.95 – 1.78 (m, 2H), 1.76 –
1.65 (m, 1H).
13
C NMR (126 MHz, CDCl3) δ 128.50, 127.97, 126.49, 74.65, 44.10, 29.52, 29.30, 12.94.