HRID1466668

反应详情

EQUATION

反应方程式

HRID 1466668 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 5-chloro-2-methoxy-benzaldehyde (prepared according to U.S. Pat. No. 4,602,035) (2.04 g, 12.0 mmol) in methanol (80 mL) was added to a stirred solution of sodium cyanide (0.90 g) and ammonium chloride (1.50 g) in aqueous ammonium hydroxide (33% solution, 30 mL) at 0° C. then warmed to room temperature for 18 hours. The mixture was evaporated to dryness, the residues partitioned between DCM and water, the organics separated, washed with brine and evaporated under vacuum to afford 2.21 g (94%) of 2-amino-2-(5-chloro-2-methoxyphenyl)acetonitrile as an orange oil. LCMS (ESI) m+H=197.2.

WORKUP

后处理

  1. customThe mixture was evaporated to dryness
  2. customthe residues partitioned between DCM and water
  3. washthe organics separated, washed with brine
  4. customevaporated under vacuum