反应详情

Add solid I2 (21.1 g, 83.1 mmol) to a biphasic mixture of 1-[benzyl-(2-methyl-allyl)-amino]-2-methyl-propan-2-ol (17.6 g, 75.4 mmol) in tert-butyl methyl ether (250 mL) and 1 M NaHCO3 (100 mL). Stir for 18 h and then add 1 M Na2S2O3 (100 mL). Dilute the mixture with additional tert-butyl methyl ether (200 mL) and separate the organic solution. Wash the organic solution with a mixture of 1 M Na2S2O3 (100 mL) and 1M NaHCO3 (100 mL). Dry, filter, and concentrate the organic solution. Dry the residue at 60° C. under vacuum to give the title compound (25.2 g, 93%) as a golden oil. 1H NMR (400 MHz, DMSO-d6): δ 7.2-7.4 (5H, m), 3.49 (1H, d), 3.47 (2H, s), 3.41 (1H, s), 2.49 (1H, d), 2.23 (1H, s), 2.20 (1H, s), 2.10 (1H, d), 1.24 (3H, s), 1.22 (3H, s), 1.15 (3H, s).

1. customseparate the organic solution
2. washWash the organic solution
3. additionwith a mixture of 1 M Na2S2O3 (100 mL) and 1M NaHCO3 (100 mL)
4. customDry
5. filtrationfilter
6. concentrationconcentrate the organic solution
7. customDry the residue at 60° C. under vacuum