HRID1287248

反应详情

EQUATION

反应方程式

HRID 1287248 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 5.7 g of 2-(m-nitroanilino)nicotinic acid ethyl ester and 50 ml of dry tetrahydrofuran was added 1.1 g of sodium amide and the solution was stirred for one hour. To this was added dropwise under cooling 2.9 g of ethyl isocyanate and this mixture was reacted at 60°C for 10 hours. After the reaction was complete, the solvent was distilled off from the mixture, and to the residue obtained was added water to precipitate a crude product. This product was collected by filtration and recrystallized from methanol to give 3.4 g of 1-(m-nitrophenyl)-3-ethylpyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione as colorless needles, melting at 210°-211°C.

WORKUP

后处理

  1. additionTo this was added dropwise
  2. customthis mixture was reacted at 60°C for 10 hours
  3. distillationthe solvent was distilled off from the mixture
  4. customto the residue obtained
  5. customto precipitate a crude product
  6. filtrationThis product was collected by filtration
  7. customrecrystallized from methanol