HRID24853

反应详情

EQUATION

反应方程式

HRID 24853 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

287 mg (0.5 mmol) of (Z)-3-{1-[4-(N-phthalimidomethylcarbonyl-N-methylamino)phenylamino]-1-phenyl-methylidene}-5-nitro-2-indolinone are suspended in 20 ml of ethanol and 20 ml of dichloromethane and after the addition of 0.3 ml of 80% hydrazine hydrate solution stirred for 18 hours at 50° C. The mixture is then cooled to ambient temperature, the insoluble matter is suction filtered and the mother liquor is concentrated by evaporation. The residue is chromatographed on silica gel (dichloromethane/methanol/ammonia=92:8:0.8) and the product is again triturated with methanol, suction filtered and dried.

WORKUP

后处理

  1. temperatureThe mixture is then cooled to ambient temperature
  2. filtrationfiltered
  3. concentrationthe mother liquor is concentrated by evaporation
  4. customThe residue is chromatographed on silica gel (dichloromethane/methanol/ammonia=92:8:0.8)
  5. customthe product is again triturated with methanol, suction
  6. filtrationfiltered
  7. customdried