HRID1064091
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
The solution of 1-Cyclohexylmethyl-4-(3,4-dichloro-phenyl)-2-methyl-5-pyridin-4-yl-pyrazolidin-3-one 0.16 g in toluene 20 mL and DMF 2 mL was treated with phenyltriethylammonium tribromide 0.22 g at room temperature, The reaction mixture was refluxed for 4 h. The reaction was quenched with sat. Na2SO3 25 mL at 0° C. The reaction mixture was extracted with dichloromethane, 3×25 mL. The combined organic phase was washed with brine, dried over anhydrous Na2SO4. After purification by flash chromatography, the title compound was obtained as light yellow solid 80 mg. MS (ES+): 416 (M+H)+.
WORKUP
后处理
- temperatureThe reaction mixture was refluxed for 4 h
- customThe reaction was quenched with sat. Na2SO3 25 mL at 0° C
- extractionThe reaction mixture was extracted with dichloromethane, 3×25 mL
- washThe combined organic phase was washed with brine
- dry with materialdried over anhydrous Na2SO4
- customAfter purification by flash chromatography