HRID1512153
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
To a mixture of 3,4,5-trifluoronitrobenzene (3.894 g, 0.022 mol) and 4-piperidone hydrochloride monohydrate (3.072 g, 0.020 mol) in chloroform (24 ml), was added triethylamine (8.3 ml, 0.06 mol) under stirring. The resulting mixture was heated and stirred at 70° C. for 7 h. After completion of the reaction (TLC), the solvent was evaporated under reduced pressure and the residue diluted with water (10 ml). The separated solid was filtered, washed with water (8 ml) followed by hexane (5 ml) to obtain yellow crystalline solid as a product, 4.8 g, 94% yield M.P.: 130-132° C.; MS: M+1=257 (MH+ 100%) for M.F.: C11H10F2N2O3
WORKUP
后处理
- temperatureThe resulting mixture was heated
- stirringstirred at 70° C. for 7 h
- customAfter completion of the reaction (TLC)
- customthe solvent was evaporated under reduced pressure
- additionthe residue diluted with water (10 ml)
- filtrationThe separated solid was filtered
- washwashed with water (8 ml)
- customto obtain yellow crystalline solid as a product