反应 #64795

反应方程式

Bis (trimethylsilyl)trifluoroacetamide

(αS)-amino-3-cyanopropanoic acid

Benzylchloroformate

→

(2S)-[[(Phenylmethoxy)carbonyl]amino]-3cyanopropanoic acid

溶剂

acetonitrile

反应条件

后处理

1. 1
   workup.STIRRINGthe reaction mixture was stirred overnight
2. 2
   浓缩concentrated in vacuo
3. 3
   workup.DISSOLUTIONdissolved in ethyl acetate (200 mL)
4. 4
   洗涤The organic solution was washed with water (2 x) and brine
5. 5
   干燥dried (Na2SO4)
6. 6
   浓缩concentrated in vacuo
7. 7
   其他Crystallization from isopropyl ether
8. 8
   其他yielded 3.82 g

实验过程

Bis (trimethylsilyl)trifluoroacetamide (9.4 mL, 35 mmol.) was added to a suspension of (αS)-amino-3-cyanopropanoic acid (2.0 g., 17.5 mmol.) in 10 mL of dry acetonitrile and the reaction mixture was stirred for 3 hours. Benzylchloroformate (2.5 mL, 17.5 mmol) was added, the reaction mixture was stirred overnight, concentrated in vacuo, and dissolved in ethyl acetate (200 mL). The organic solution was washed with water (2 x) and brine, dried (Na2SO4), and concentrated in vacuo. Crystallization from isopropyl ether yielded 3.82 g. of the title A product.

来源