HRID65193

反应详情

EQUATION

反应方程式

HRID 65193 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.8 g of 4-morpholino-3-trifluoromethylbenzoylpropionic acid-morpholineamide together with 2.2 ml of hydrazine hydrate and 90 ml of 50% acetic acid are refluxed for 1 hour. The reaction mixture is cooled, concentrated in a rotary evaporator, and a small amount of water is added; the pH-value is adjusted to 6 with a 2 N sodium carbonate solution, and the mixture is extracted with methylene chloride. The methylene chloride extracts are washed with water, dried over sodium sulfate and concentrated by evaporation. From the residue is obtained, by recrystallisation from ethanol/petroleum ether, 6-(3-trifluoromethyl-4-morpholino-phenyl)-4,5-dihydro-3(2H)-pyridazinone, m.p. 163°-166° C.

WORKUP

后处理

  1. temperatureThe reaction mixture is cooled
  2. concentrationconcentrated in a rotary evaporator
  3. additiona small amount of water is added
  4. extractionthe mixture is extracted with methylene chloride
  5. washThe methylene chloride extracts are washed with water
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated by evaporation