HRID1243307

反应详情

EQUATION

反应方程式

HRID 1243307 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

10.5 g (30.0 mmol) of 1-acetyl-3-(1-ethoxy-1-phenylmethylene)-6-methoxycarbonyl-2-indolinone (for preparation see WO 01/27081 mentioned above) and 8.60 g (33.0 mmol) N-[(4-methyl-piperazin-1-yl)-methylcarbonyl]-N-methyl-p-phenylenediamine (for preparation see WO 01/27081 mentioned above) are dissolved in 80 mL of dimethylformamide and stirred for 1 hour at 80° C. After cooling 6.50 mL of piperidine are added and the mixture is stirred for another two hours at ambient temperature. Water is added, the precipitate formed is suction filtered and washed with a little water. The residue is suspended in 200 mL of methanol, suction filtered and washed with cold water and diethyl ether. The substance is dried in vacuo at 110° C.

WORKUP

后处理

  1. additionare added
  2. stirringthe mixture is stirred for another two hours at ambient temperature
  3. customthe precipitate formed
  4. filtrationfiltered
  5. washwashed with a little water
  6. filtrationsuction filtered
  7. washwashed with cold water and diethyl ether
  8. customThe substance is dried in vacuo at 110° C.