반응 #64795

반응 방정식

Bis (trimethylsilyl)trifluoroacetamide

(αS)-amino-3-cyanopropanoic acid

Benzylchloroformate

→

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

용매

acetonitrile

반응 조건

후처리

1. 1
   workup.STIRRINGthe reaction mixture was stirred overnight
2. 2
   농축concentrated in vacuo
3. 3
   workup.DISSOLUTIONdissolved in ethyl acetate (200 mL)
4. 4
   세척The organic solution was washed with water (2 x) and brine
5. 5
   건조dried (Na2SO4)
6. 6
   농축concentrated in vacuo
7. 7
   기타Crystallization from isopropyl ether
8. 8
   기타yielded 3.82 g

실험 절차

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.

출처