HRID1859681

反应详情

EQUATION

反应方程式

HRID 1859681 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Concentrated HCl (45 mL) was added to a solution of 3-[acetyl-(3,5-dichlorophenyl)-amino]-4-methoxybenzoic acid methyl ester (11.46 g, 31.12 mmol) in a mixture of tetrahydro-furan (75 mL) and methanol (75 mL). The reaction was heated to reflux. After 3 days, the solvent was removed in vacuo and the residue was dissolved in ethyl acetate and dried (MgSO4). The ethyl acetate was removed under reduced pressure to give the product (2.4 g); m.p. 134-135° C. after chromatography on silica gel in ethyl acetate followed by recrystallization from ether/hexane 1:9.

WORKUP

后处理

  1. temperatureThe reaction was heated to reflux
  2. customthe solvent was removed in vacuo
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. dry with materialdried (MgSO4)
  5. customThe ethyl acetate was removed under reduced pressure