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
- 20 °C
PROCEDURE
实验过程
4-Amino-7-trifluoromethylquinoline (120 mg, 0.56 mmol), triethylamine (170 mg, 1.7 mmol) and CHCl3 (4 mL) were charged in a 10 ml round-bottomed flask equipped with a magnetic stirrer. 5-Bromovaleryl chloride (140 mg, 0.7 mmol in CHCl3 (2 mL) were added and the reaction mixture was stirred for 15 h at 20° C. The reaction mixture was poured in 10 mL of H2O and extracted with CH2Cl2 (100 mL). The organic layer was washed with brine (2×10 mL), dried over MgSO4, filtered and evaporated at 30° C. to dryness. The crude compound was purified by column chromatography (SiO2; CH2Cl2:MeOH=99.5:0.5 to 98:2) to give after evaporation 5-bromo-N-(7-(trifluoromethyl)quinolin-4-yl)pentanamide 32 (190 mg, 90% yield) as a beige solid.
WORKUP
后处理
- customequipped with a magnetic stirrer
- extractionextracted with CH2Cl2 (100 mL)
- washThe organic layer was washed with brine (2×10 mL)
- dry with materialdried over MgSO4
- filtrationfiltered
- customevaporated at 30° C. to dryness
- customThe crude compound was purified by column chromatography (SiO2; CH2Cl2:MeOH=99.5:0.5 to 98:2)
- customto give