HRID2094661
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
The compound of step 1 (900 mg, 2.85 mmol) was dissolved in 1,3-dimethyl-2-imidazolidinone (6 ml), and sodium methanethiolate (0.23 g, 3.29 mmol) was added. The mixture was reacted at room temperature for 60 h, then partitioned between a saturated sodium chloride solution and EA, and the aqueous phase extracted with EA. The organic extracts were dried over sodium sulfate, filtered and evaporated to dryness. The residue was purified by silica gel chromatography (HEP/EA gradient) to give 600 mg of the title compound.
WORKUP
后处理
- customThe mixture was reacted at room temperature for 60 h
- custompartitioned between a saturated sodium chloride solution and EA
- extractionthe aqueous phase extracted with EA
- dry with materialThe organic extracts were dried over sodium sulfate
- filtrationfiltered
- customevaporated to dryness
- customThe residue was purified by silica gel chromatography (HEP/EA gradient)