HRID25329

反应详情

EQUATION

反应方程式

HRID 25329 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

54.3 g of methyl 3-nitro-benzoate and 29.0 g of methyl chioroacetate are dissolved in 100 ml of dimethylformamide and this solution is added dropwise at −10° C. to a solution of 78.5 g of potassium tert.butoxide in 500 ml of dimethylformamide. The mixture is stirred for another 10 minutes at ambient temperature and after this time the solution is poured onto 350 ml of concentrated hydrochloric acid in 2 l of iced water. The solution is stirred for 0.5 hours and the precipitate obtained is suction filtered and washed with water. The product is recrystallised from 150 ml of methanol and dried in vacuo at 40° C. Yield: 48.3 g (51% of theoretical), contains about 20% of methyl 6-methoxycarbonylmethyl-3-nitro-benzoate

WORKUP

后处理

  1. stirringThe solution is stirred for 0.5 hours
  2. customthe precipitate obtained
  3. filtrationfiltered
  4. washwashed with water
  5. customThe product is recrystallised from 150 ml of methanol
  6. customdried in vacuo at 40° C