HRID36537

反应详情

EQUATION

反应方程式

HRID 36537 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

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×) and brine, dried (Na2SO4), and concentrated in vacuo. Crystallization from isopropyl ether yielded 3.82 g. of the title A product.

WORKUP

后处理

  1. stirringthe reaction mixture was stirred overnight
  2. concentrationconcentrated in vacuo
  3. dissolutiondissolved in ethyl acetate (200 mL)
  4. washThe organic solution was washed with water (2×) and brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated in vacuo
  7. customCrystallization from isopropyl ether
  8. customyielded 3.82 g