HRID867181

反应详情

EQUATION

反应方程式

HRID 867181 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Formic acid (140 ml) was added dropwise to acetic anhydride (200 ml) cooled on an ice bath. The solution was heated at 50° C. for 15 minutes and then cooled to 5° C. To the solution, 5,8-dihydro-2-(1-piperazinyl)-5-oxopyrido[2,3-d] pyrimidine-6-carboxylic acid (70 g) was added. The mixture was heated at 80° C. for 3 hours and then cooled. The crystals precipitated were collected by filtration and washed with ethyl ether to give 5,8-dihydro-2-(4-formyl-1-piperazinyl)-5-oxopyrido[2,3-d]pyrimidine-6-carboxylic acid (72.5 g). m.p. above 300° C.

WORKUP

后处理

  1. temperaturecooled on an ice bath
  2. temperaturecooled to 5° C
  3. temperatureThe mixture was heated at 80° C. for 3 hours
  4. temperaturecooled
  5. customThe crystals precipitated
  6. filtrationwere collected by filtration
  7. washwashed with ethyl ether