HRID1159186

反应详情

EQUATION

反应方程式

HRID 1159186 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 3-(4-chlorophenyl)-propionaldehyde (0.74 g, 4.39 mmol) was added zinc iodide (0.07 g, 0.22 mmol) and trimethylsilyl cyanide (0.522 g, 5.27 mmol) with caution (exothermic reaction). After stirring the mixture at room temperature for 20 min a solution of ammonia in methanol (7N, 4.4 ml, 31 mmol) was added and stirring was continued overnight. The solvent was evaporated and the residue was purified by chromatography (column: Isolute® Flash-NH2 from Separtis; eluent:heptane/ethyl acetate=2:1) to yield a light yellow liquid (0.43 g, 50%); MS (ISP): 195.3 ((M+H)+).

WORKUP

后处理

  1. customwith caution (exothermic reaction)
  2. additionwas added
  3. customThe solvent was evaporated
  4. customthe residue was purified by chromatography (column: Isolute® Flash-NH2 from Separtis; eluent:heptane/ethyl acetate=2:1)