反応 #64795

反応方程式

Bis (trimethylsilyl)trifluoroacetamide

(αS)-amino-3-cyanopropanoic acid

Benzylchloroformate

→

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

溶媒

acetonitrile

反応条件

後処理

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

実験手順

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.

出典