HRID65193
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction mixture is cooled
- concentrationconcentrated in a rotary evaporator
- additiona small amount of water is added
- extractionthe mixture is extracted with methylene chloride
- washThe methylene chloride extracts are washed with water
- dry with materialdried over sodium sulfate
- concentrationconcentrated by evaporation