HRID1007371

反应详情

EQUATION

反应方程式

HRID 1007371 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

2.0 g of 2,4-dinitrophenylacetic acid (prepared according to J: Chem. Soc. 1948, 1717) are dissolved in 40 ml ethanol and 6.0 ml of conc. hydrochloric acid and 4.1 g of tin-(II)-chloride-dihydrate are added in batches at ambient temperature. The mixture is stirred for 12 hours at ambient temperature and for 4 hours at 60° C. After cooling another 2.0 g of tin-(II)-chloride-dihydrate are added and the mixture is stirred for another 12 hours at ambient temperature. The reaction mixture is diluted with water, extracted with methylene chloride and the organic phase is dried over sodium sulphate. After elimination of the solvent the residue is triturated with ether and the precipitate is filtered off.

WORKUP

后处理

  1. additionare added
  2. stirringthe mixture is stirred for another 12 hours at ambient temperature
  3. extractionextracted with methylene chloride
  4. dry with materialthe organic phase is dried over sodium sulphate
  5. customAfter elimination of the solvent the residue is triturated with ether
  6. filtrationthe precipitate is filtered off