HRID1287245

反应详情

EQUATION

反应方程式

HRID 1287245 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.8 g of 1-(m-nitrophenyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione was dissolved in 30 ml of dry dimethylformamide. To the solution was added 0.6 g of about 50 % sodium hydride, and stirring was performed for 30 minutes. To the mixture was further added 3.5 g of diethylsulfite and the whole was reacted for 2 hours at room temperature. After the reaction was finished, the solvent was distilled off from the mixture under reduced pressure. To the residue thus obtained was added water to precipitate a crude product. This product was recrystallized from methanol to yield 2.7 g of 1-(m-nitrophenyl)-3-ethylpyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione as pale yellow prisms, melting at 210°-211°C.

WORKUP

后处理

  1. customthe whole was reacted for 2 hours at room temperature
  2. distillationthe solvent was distilled off from the mixture under reduced pressure
  3. customTo the residue thus obtained
  4. customto precipitate a crude product
  5. customThis product was recrystallized from methanol