HRID1382968

反应详情

EQUATION

反应方程式

HRID 1382968 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of the tetrabutylammonium salt of 4-amino-5- chloro-N-[2-(diethylamino)ethyl]-2-hydroxybenzamide (3.45 g, 6.5 mmoles) and 1-chloro-3-phenyl-2-propanone (1.1 g, 6.5 mmoles) in acetonitrile was stirred for 18 hours at 20°. After removal of the acetonitrile at reduced pressure, the residue was treated with water and extracted with methylene chloride. The residue, after concentration of the extracts, was chromatographed on alumina (grade III) using ethyl acetate for elution. Combination of the appropriate fractions gave 1.1 g of product which was recrystallized from ethyl acetate to give the title compound, mp. 138°-139°.

WORKUP

后处理

  1. customAfter removal of the acetonitrile at reduced pressure
  2. additionthe residue was treated with water
  3. extractionextracted with methylene chloride
  4. customThe residue, after concentration of the extracts, was chromatographed on alumina (grade III)
  5. washfor elution