反应详情

To chlorosulfonylisocyanate (10.3 g) was added t-butyl alcohol (6.96 ml) in dichloromethane (30 ml) under ice-water cooling and the mixture was stirred at ambient temperature for 0.5 hour. The solution was added into a mixture of N-hydroxysuccinimide (8.38 g) and pyridine (6.47 ml) in dichloromethane (150 ml) under ice-water cooling and the mixture was stirred at 0° C. for 1 hour. The solution was washed with 0.1N hydrochloric acid, water and brine, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by silica gel column chromatography eluting with a mixture of chloroform and methanol (200:1, 100:1, 200:3, 50:1) to give N-(t-butoxycarbonylamino-sulfonyloxy)succinimide as colorless oil (2.93 g).

1. stirringthe mixture was stirred at 0° C. for 1 hour
2. washThe solution was washed with 0.1N hydrochloric acid, water and brine
3. dry with materialdried over magnesium sulfate
4. customevaporated in vacuo
5. customThe residue was purified by silica gel column chromatography
6. washeluting with a mixture of chloroform and methanol (200:1, 100:1, 200:3, 50:1)