反应详情

25 g of ammonia gas and 50 g of hydrogen sulfide gas were successively dissolved in 230 ml of methanol with ice-cooling and stirring. To this was added 71.45 g of (tert-butoxycarbonylamino)acetonitrile, and the mixture was stirred overnight at room temperature. The reaction solution was cooled with ice. To this was slowly added 500 ml of water, and the mixture was stirred for an additional 2 hours with ice- cooling. The crystals precipitated were collected by filtration, washed with 300 ml of cold water, and then dried under reduced pressure to give 65.88 g of (tert-butoxycarbonyl-amino)acetothioamide as colorless crystals.

1. temperaturecooling
2. stirringthe mixture was stirred overnight at room temperature
3. temperatureThe reaction solution was cooled with ice
4. stirringthe mixture was stirred for an additional 2 hours with ice-
5. temperaturecooling
6. customThe crystals precipitated
7. filtrationwere collected by filtration
8. washwashed with 300 ml of cold water
9. customdried under reduced pressure