反应 #710534

反应方程式

Methanesulfonic acid

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

triethylamine

→

titled compound

(S)-tert-leucine

溶剂

methylene chloride

反应条件

后处理

1. 1
   其他a solid was precipitated
2. 2
   其他The 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
   其他Thereafter, the solid was separated by filtration under reduced pressure
6. 6
   洗涤The solid was washed with methylene chloride (5 mL)
7. 7
   其他drying

实验过程

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%).

来源