HRID328125

反应详情

EQUATION

反应方程式

HRID 328125 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3.0 g of 2-(m-nitroanilino)-N-allylbenzamide and 25 ml of tetrahydrofuran was added 1.1 g of 50 % sodium hydride, and the whole was stirred for 30 minutes at room temperature. To this was added dropwise under cooling 16 g of 30 % phosgene-toluene solution, and the mixture was stirred for one hour at room temperature and then refluxed for 2 hours. After the reaction was finished, the solvent was distilled off from the resulting mixture, and to the residue obtained was added water to precipitate a crude product. This product was recrystallized from methanol to yield 2.8 g of 1-(m-nitrophenyl)-3-allylquinazoline-2,4(1H, 3H)-dione as colorless needles, melting at 164°-166° C.

WORKUP

后处理

  1. additionTo this was added dropwise
  2. stirringthe mixture was stirred for one hour at room temperature
  3. temperaturerefluxed for 2 hours
  4. distillationthe solvent was distilled off from the resulting mixture
  5. customto the residue obtained
  6. customto precipitate a crude product
  7. customThis product was recrystallized from methanol