HRID1944688
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 160 °C
PROCEDURE
实验过程
A mixture of 5-bromo-2-(methylthio)benzothiazole (200 mg, 0.77 mmol), 1-isopropylpiperazine (985 mg, 7.7 mmol) and pyridine (610 mg, 7.7 mmol) was heated at 160° C. for 36 h. The reaction mixture was concentrated under reduced pressure and the residue was extracted with dichloromethane (3×10 mL). The combined organic extracts were washed with brine, dried (Na2SO4) and concentrated. The residue was purified by column chromatography on silica gel (eluent: 2% EtOAc in Petroleum ether) to give 200 mg (77%) of 5-bromo-2-(4-isopropylpiperazin-1-yl)benzothiazole.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under reduced pressure
- extractionthe residue was extracted with dichloromethane (3×10 mL)
- washThe combined organic extracts were washed with brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated
- customThe residue was purified by column chromatography on silica gel (eluent: 2% EtOAc in Petroleum ether)