HRID328124

反应详情

EQUATION

反应方程式

HRID 328124 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 2.9 g of 2-(m-nitroanilino)-N-ethylbenzamide and 25 ml of tetrahydrofuran was added 1.0 g of 50 % sodium hydride, and stirring was performed for 30 minutes at room temperature. To this was added dropwise under cooling 5.4 g of ethyl chlorocarbonate, and the mixture was allowed to stand for one hour at room temperature and then refluxed for 10 hours. After the reaction was complete, the solvent was evaporated from the reaction mixture under reduced pressure, and to the residue obtained was added water to prepicpitate a crude product. This product was recrystallized from methanol to give 2.5 g of 1-(m-nitrophenyl)-3-ethylquinazoline-2,4(1H, 3H)-dione as colorless prisms, melting at 193°-194° C.

WORKUP

后处理

  1. additionTo this was added dropwise
  2. waitto stand for one hour at room temperature
  3. temperaturerefluxed for 10 hours
  4. customthe solvent was evaporated from the reaction mixture under reduced pressure
  5. customto the residue obtained
  6. customThis product was recrystallized from methanol