HRID499097
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
- 150 °C
PROCEDURE
实验过程
To a solution of 6-bromoquinoline (700 mg) in dimethylacetamide (3 ml) was added sodium thiomethoxide (1.9 g, 26.96 mmol). The mixture was heated at 150° C. for 2 hours, then cooled to ambient and diluted with 1M HCl/ethyl acetate. The organic layer was removed and the aqueous layer extracted with further ethyl acetate. The combined extracts were washed with water, then brine, dried (MgSO4), filtered and concentrated. The crude thiol (500 mg) was used directly without further purification; MS ES+, ES− 174.13
WORKUP
后处理
- temperaturecooled
- customThe organic layer was removed
- extractionthe aqueous layer extracted with further ethyl acetate
- washThe combined extracts were washed with water
- dry with materialbrine, dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- customThe crude thiol (500 mg) was used directly without further purification