HRID347688
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
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
A mixture of 0.21 g (0.44 mmol) 6′-chloro-2-methyl-[3,4′]bipyridinyl-3′-carboxylic acid (3,5-bis-trifluoromethyl-benzyl)-methyl-amide and 1.0 ml (9.0 mmol) 1-methylpiperazine was heated at 120° C. for 2 h. After cooling to room temperature the mixture was diluted with dichloromethane and washed with water. The aqueous layer was extracted with dichloromethane. The combined organic layers were dried over sodium sulfate and concentrated in vacuo to give 0.25 g of crude product. Flash chromatography gave 0.17 g (70%) of the title compound. MS m/e (%): 552 (M+H+, 100)
WORKUP
后处理
- temperatureAfter cooling to room temperature the mixture
- washwashed with water
- extractionThe aqueous layer was extracted with dichloromethane
- dry with materialThe combined organic layers were dried over sodium sulfate
- concentrationconcentrated in vacuo
- customto give 0.25 g of crude product