HRID347692
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
- 140 °C
PROCEDURE
实验过程
A mixture of 0.16 g (0.30 mmol) 2-(3,5-bis-trifluoromethyl-phenyl)-N-(6′-chloro-2-methyl-[3,4′]bipyridinyl-3′-yl)-N-methyl-isobutyramide, 0.67 ml (6.0 mmol) 1-methylpiperazine and 2 mg (0.02 mmol) 4-(N,N-dimethylamino)pyridine was heated at 140° C. over night. After cooling to room temperature the mixture was diluted with tert-butyl methyl ether and washed with water. The aqueous layer was extracted with two portions of tert-butyl methyl ether. The combined organic layers were dried over sodium sulfate and concentrated in vacuo. Flash chromatography gave 0.16 g (93%) of the title compound.
WORKUP
后处理
- temperatureAfter cooling to room temperature the mixture
- washwashed with water
- extractionThe aqueous layer was extracted with two portions of tert-butyl methyl ether
- dry with materialThe combined organic layers were dried over sodium sulfate
- concentrationconcentrated in vacuo