反应详情

温度

177.5 °C

1 mol of an ephedrine, 1.025 mol of ammonium sulfamate, 3 mol of urea and the proton-donating compound were introduced into 200 ml of NMP. The reaction mixture was heated to 175 to 180° C. and stirred at this temperature for 2.5 h. It was then cooled to 130° C. and, at this temperature, water was added dropwise to the reaction mixture. Two phases formed. The lower phase was removed at 95° C. The upper phase was further cooled initially to 65° C. Crystals formed at this temperature. It was cooled further to 10° C. and stirred at this temperature for 1 h. The crystals were filtered off with suction and washed twice with cold water. The solid was dried in vacuo at RT overnight.

1. additionwas added dropwise to the reaction mixture
2. customTwo phases formed
3. customThe lower phase was removed at 95° C
4. temperatureThe upper phase was further cooled initially to 65° C
5. customCrystals formed at this temperature
6. temperatureIt was cooled further to 10° C.
7. stirringstirred at this temperature for 1 h
8. filtrationThe crystals were filtered off with suction
9. washwashed twice with cold water
10. customThe solid was dried in vacuo at RT overnight