HRID993053

反应详情

EQUATION

反应方程式

HRID 993053 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-[3-(4-Methoxyphenyl)propyl]barbituric Acid (2.5 g), N-bromosuccinimide (2 g) and dibenzoyl peroxide (catalytic amount) in 110 ml of carbon tetrachloride is refluxed for about 1 hour, then the solid which separated is filtered. The solid is redissolved in ethyl acetate and filtered through a silica gel cake in order to eliminate the succinimide residue. The organic phase is then concentrated to dryness and the residue is crystallized from diethylether/carbon tetrachloride mixture. A pale yellow solid separates which is filtered and dried under vacuum at 60° C. to give 2.8 g of the product, m.p. 113-114° C.

WORKUP

后处理

  1. temperatureis refluxed for about 1 hour
  2. customthe solid which separated
  3. filtrationis filtered
  4. dissolutionThe solid is redissolved in ethyl acetate
  5. filtrationfiltered through a silica gel cake in order
  6. concentrationThe organic phase is then concentrated to dryness
  7. customthe residue is crystallized from diethylether/carbon tetrachloride mixture
  8. filtrationA pale yellow solid separates which is filtered
  9. customdried under vacuum at 60° C.