HRID358661

反应详情

EQUATION

反应方程式

HRID 358661 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Triethylamine (362.8 ml) was added to a stirred mixture of benzoic acid (239.1 g) and dichloromethane (1120 ml) at 0° and the resultant solution was added dropwise over a period of 1 hour to the solution of 2'-(2-chloroacetyl)-N-methylformanilide under nitrogen whilst maintaining the temperature below 5°. The resulting solution was stirred overnight at ambient temperature, washed with water (2×1250 ml), dried over magnesium sulphate and the solvent removed by distillation at 50° to give a solid residue. Trituration with petroleum ether (b.p. 60°-80°, 1 1) gave the novel compound 2-[2-(N-methylformamido)phenyl]-2-oxoethyl benzoate, m.p. 100°-102°.

WORKUP

后处理

  1. temperaturewhilst maintaining the temperature below 5°
  2. washwashed with water (2×1250 ml)
  3. dry with materialdried over magnesium sulphate
  4. customthe solvent removed by distillation at 50°
  5. customto give a solid residue