HRID1018023

反应详情

EQUATION

反应方程式

HRID 1018023 反应方程式

PROCEDURE

实验过程

Dimethylformamide (2.71 g, 0.037 moles) was added to a well stirred and cooled material of triphosgene (10.99 g, 0.037 moles) at 4° C. in 30 minutes in an ice bath followed by N-benzyl-N-(1-Propenyl)acetamide (1 g, 0.005 moles) at the temperature. The reaction mixture was further continued for 2 hours at 25° C. The ice cold bath was removed and heated to75° C. for 5 hours. Work up procedure was carried out according to the procedure of example 1. The obtained residue was subjected to chromatographic purification on silica gel to give 2-chloro-5-methylpyridine-3-carbaldeyde in 92% yield.

WORKUP

后处理

  1. customThe ice cold bath was removed
  2. temperatureheated to75° C
  3. waitfor 5 hours
  4. customThe obtained residue was subjected to chromatographic purification on silica gel