HRID14262
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
A solution of 7-bromo-1-chloroisoquinoline (750 mg, 3.09 mmol) in N-methylbutylamine (7.0 mL) was heated at 65° C. in a sealed tube for 18 h. The reaction mixture was concentrated under reduced pressure. The residue was diluted with chloroform and washed with saturated sodium bicarbonate, dried (sodium sulfate), filtered, and concentrated under reduced pressure to yield a brown oil. Purification by flash column chromatography (silica, 3:1 hexanes/diethyl ether) provided 7-bromo-N-butyl-N-methylisoquinolin-1-amine (730 mg): ESI MS m/z 293 [M+H]+.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under reduced pressure
- additionThe residue was diluted with chloroform
- washwashed with saturated sodium bicarbonate
- dry with materialdried (sodium sulfate)
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customto yield a brown oil
- customPurification by flash column chromatography (silica, 3:1 hexanes/diethyl ether)