HRID1460679

反应详情

EQUATION

反应方程式

HRID 1460679 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

20 Grams of 6-[4-(2-benzoylethyl)-1-piperazinylcarbonyl]-3,4-dihydrocarbostyril and 5.33 g of hydroxylamine hydrochloride were dispersed in 40 ml of pyridine and the suspension was stirred at 100° C. for 4 hours. After the reaction was completed, the reaction mixture was poured into water and then extracted with chloroform, the extract was dried with anhydrous potassium carbonate, then the solvent was removed by evaporation. The thus obtained residue was purified by means of a silica gel column chromatography (eluent: dichloromethane:methanol =50:1), then recrystallized from ethanol to yield 8.79 g of 6[-4-(3-hydroxyimino-3-phenylpropyl)-1-piperazinylcarbonyl]-3,4-dihydrocarbostyril 1/2-hydrate. White powdery substance. Melting point: 167° C.-169° C. (decomp.)

WORKUP

后处理

  1. extractionextracted with chloroform
  2. dry with materialthe extract was dried with anhydrous potassium carbonate
  3. customthe solvent was removed by evaporation
  4. customThe thus obtained residue was purified by means of a silica gel column chromatography (eluent: dichloromethane:methanol =50:1)
  5. customrecrystallized from ethanol