HRID624885

反应详情

EQUATION

反应方程式

HRID 624885 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of (S)-2-(tert-butoxycarbonylamino)-3-cyclopropylpropanoic acid (CAN 89483-06-7, 10 g, 44 mmol), di-tert-butyl dicarbonate (CAN:24424-99-5, 14.28 g, 66 mmol) and pyridine (2.4 mL) in acetonitrile (200 mL) was stirred at room temperature for 20 min. Ammonia (10 mL) was added dropwise for 20 min. The resulting reaction mixture was stirred for 4 h. During removal of most of the solvent under reduced pressure the product precipitated and the solid was filtered off and washed with acetonitrile (20 mL). The solid was dried under reduced pressure to give the title compound (7.73 g, 78%) as white solid; MS (EI): m/e 251.2 [M+Na]+.

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. stirringwas stirred for 4 h
  3. customDuring removal of most of the solvent under reduced pressure the product
  4. customprecipitated
  5. filtrationthe solid was filtered off
  6. washwashed with acetonitrile (20 mL)
  7. customThe solid was dried under reduced pressure