반응 #710535

반응 방정식

Methanesulfonic acid

(S)—N-(tert-butoxycarbonyl)-2-methylproline

triethylamine

→

titled compound

(S)-2-methylproline

용매

1,2-dichloroethane

반응 조건

후처리

1. 1
   기타a solid was precipitated
2. 2
   기타The solid was sufficiently precipitated
3. 3
   workup.STIRRINGthe solution was stirred at 25° C. for 30 minutes
4. 4
   workup.STIRRINGfurther stirred at 25° C. for 2 hours
5. 5
   기타Thereafter, the solid was then separated by filtration under reduced pressure
6. 6
   세척The solid was washed with 1,2-dichloroethane (0.2 mL)
7. 7
   기타drying

실험 절차

Methanesulfonic acid (252 mg, 2.6 mmol) was added to a solution of (S)—N-(tert-butoxycarbonyl)-2-methylproline (500 mg, 2.2 mmol) and 1,2-dichloroethane (2.53 g), and the mixture was stirred at 25° C. for 3 hours. When triethylamine (265 mg, 2.6 mmol) was added thereto, a solid was precipitated. The solid was sufficiently precipitated, and then the solution was stirred at 25° C. for 30 minutes and further stirred at 25° C. for 2 hours. Thereafter, the solid was then separated by filtration under reduced pressure. The solid was washed with 1,2-dichloroethane (0.2 mL), and then was subjected to vacuum drying. Thereby, the titled compound was produced as a white solid (197 mg, yield of 69%).

출처