HRID328131

反应详情

EQUATION

反应方程式

HRID 328131 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.0 g of 2-(m-nitroanilino)-N-allylbenzamide was dissolved in 20 ml of tetrahydrofuran. To the solution was added 1.0 g of approximately 50 % sodium hydride and stirring was performed for 30 minutes. To this was added dropwise under cooling 4.6 g of m-chlorophenyl isocyanate, and the mixture was stirred for one hour, and then refluxed for 5 hours. After the reaction was complete, the solvent was distilled off from the resulting mixture. The residue thus obtained was recrystallized from methanol to give 2.3 g of 1-(m-nitrophenyl)-3-allylquinazoline-2,4(1H, 3H)-dione as colorless needles, melting at 165°-166° C.

WORKUP

后处理

  1. additionTo this was added dropwise
  2. stirringthe mixture was stirred for one hour
  3. temperaturerefluxed for 5 hours
  4. distillationthe solvent was distilled off from the resulting mixture
  5. customThe residue thus obtained
  6. customwas recrystallized from methanol