반응 #710534

반응 방정식

Methanesulfonic acid

(S)—N-(tert-butoxycarbonyl)-tert-leucine

triethylamine

→

titled compound

(S)-tert-leucine

용매

methylene chloride

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 30 minutes
5. 5
   기타Thereafter, the solid was separated by filtration under reduced pressure
6. 6
   세척The solid was washed with methylene chloride (5 mL)
7. 7
   기타drying

실험 절차

Methanesulfonic acid (576 mg, 6 mmol) was added to a solution of (S)—N-(tert-butoxycarbonyl)-tert-leucine (1155 mg, 5 mmol) and methylene chloride (5 mL), and the mixture was stirred at 25° C. for 3 hours. When triethylamine (708 mg, 7 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 30 minutes. Thereafter, the solid was separated by filtration under reduced pressure. The solid was washed with methylene chloride (5 mL), and then was subjected to vacuum drying. Thereby, the titled compound was produced as a white solid (514 mg, yield of 75%).

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