HRID1380070

反应详情

EQUATION

反应方程式

HRID 1380070 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-phenylhydantoin (5 g, 28.3 mmoles), 85% potassium hydroxide (2.06 g, 31.2 mmoles), 1,2-dibromoethane (11.72 g, 62.4 mmoles) and potassium iodide (catalytic amounts) in 100 ml of ethanol was refluxed for 67 hours. The solid was filtered, the mother liquors were evaporated and the crude product was purified by silica gel column chromatography eluting with increasing mixtures of ethyl acetate in hexane. By crystallization from acetone/hexane 1.56 g of the title compound were obtained, m.p. 146°-147° C.

WORKUP

后处理

  1. temperaturewas refluxed for 67 hours
  2. filtrationThe solid was filtered
  3. customthe mother liquors were evaporated
  4. customthe crude product was purified by silica gel column chromatography
  5. washeluting with increasing mixtures of ethyl acetate in hexane
  6. customBy crystallization from acetone/hexane 1.56 g of the title compound
  7. customwere obtained