HRID2379698

反应详情

EQUATION

反应方程式

HRID 2379698 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

180.5 g (0.4 mol) of finely divided compound from Example I are intensively stirred under reflux for 5 h in 2.6 l of 2N HCl using a mechanical stirrer. The mixture is then neutralised with NaHCO3 and extracted several times with ethyl acetate, and the extracts are dried. 37.6 g of the title compound are obtained by crystallisation. Chromatography of the mother liquor (silica gel, toluene→toluene/ethyl acetate 2:1) yields a further 23.14 g of the title compound. Total yield: 60% M.p.: 136° C.

WORKUP

后处理

  1. extractionextracted several times with ethyl acetate
  2. customthe extracts are dried