HRID328120

反应详情

EQUATION

反应方程式

HRID 328120 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 2.8 g of 1-(m-nitrophenyl)quinazoline-2,4(1H, 3H)-dione and 30 ml of dimethylformamide was added 0.6 g of approximately 55 % sodium hydride, and the solution was stirred for 20 minutes at room temperature. To this was added 2.2 g of dimethyl sulfite and stirring was further continued for 4 hours at room temperature. After the reaction was complete, the solvent was removed from the reaction mixture by distillation under reduced pressure. The residue thus obtained was mixed with water to precipitate a crude product. This product was recrystallized from methanol to afford 2.8 g of 1-(m-nitrophenyl)-3-methylquinazoline-2,4(1H, 3H)-dione as colorless needles, melting at 242°-243° C.

WORKUP

后处理

  1. stirringstirring
  2. waitwas further continued for 4 hours at room temperature
  3. customthe solvent was removed from the reaction mixture by distillation under reduced pressure
  4. customThe residue thus obtained
  5. customto precipitate a crude product
  6. customThis product was recrystallized from methanol