HRID1492365
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
To a solution of 2,6-dichloro-4-nitropyridine (3.8 g; 0.02 mol) in dimethylformamide (50 ml) cooled with an ice-bath was sodium thiomethoxide (1.4 g; 0.02 mol) slowly added. After stirring for 3 hours, the reaction mixture was quenched with water (300 ml) and extracted 3 times each with a hexane/ethyl acetate mixture (100 ml; 1/1). The combined extracts were dried with anhydrous magnesium sulphate and the solvent was removed in vacuo. Purification by silica gel flash column chromatography afforded 2,6-dichloro-4-methylthiopyridine (2.9 g; 74%) as a colorless oil.
WORKUP
后处理
- additionslowly added
- customthe reaction mixture was quenched with water (300 ml)
- extractionextracted 3 times each with a hexane/ethyl acetate mixture (100 ml; 1/1)
- dry with materialThe combined extracts were dried with anhydrous magnesium sulphate
- customthe solvent was removed in vacuo
- customPurification by silica gel flash column chromatography