HRID432052

反应详情

EQUATION

反应方程式

HRID 432052 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

27 g of acetyl chloride (0.344 mol) are added dropwise to a mixture of 245 ml of methanol and 245 ml of acetone. 20 g (0.123 mol) of benzofuran-2,3-dione 2-oxime are dissolved in this mixture and the mixture is subsequently heated under reflux for 1 hour. The solvent is distilled off under reduced pressure, the residue is poured into water, the product is extracted with diethyl ether, the organic phase is dried over sodium sulphate and the solvent is distilled off under reduced pressure. This gives 20.8 g of crude product which, according to HPLC, contains 92.4% methyl 2-hydroxyphenylglyoxylate of log p=1.87.

WORKUP

后处理

  1. temperaturethe mixture is subsequently heated
  2. temperatureunder reflux for 1 hour
  3. distillationThe solvent is distilled off under reduced pressure
  4. additionthe residue is poured into water
  5. extractionthe product is extracted with diethyl ether
  6. dry with materialthe organic phase is dried over sodium sulphate
  7. distillationthe solvent is distilled off under reduced pressure