HRID1294566

反应详情

EQUATION

反应方程式

HRID 1294566 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

1.37 g (9.85 mmol) 2-amino-6-fluoro-benzaldehyde are combined with 20 ml acetic anhydride and heated to 70° C. for 4 h. Then the reaction mixture is stirred into 200 ml dist. water, adjusted to pH 7 with Na2CO3 and extracted three times with 50 ml of ethyl acetate. Then the organic phase is dried with MgSO4, the solvent is eliminated in vacuo. The crude product is purified by column chromatography. The carrier material used is silica gel and the eluant used is a mixture of cyclohexane:ethyl acetate (80:20).

WORKUP

后处理

  1. extractionextracted three times with 50 ml of ethyl acetate
  2. dry with materialThen the organic phase is dried with MgSO4
  3. customThe crude product is purified by column chromatography
  4. additiona mixture of cyclohexane:ethyl acetate (80:20)