HRID62873
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
- -78 °C
PROCEDURE
实验过程
After 2-isopropylsulfanyl-6-methyl-nicotinic acid methyl ester (105 mg, 0.46 mmol) was dissolved in THF (3 mL), KHMDS (1 mL, 0.51 mmol) was added slowly thereto at −78° C., and the mixture was stirred for 30 minutes. MeI (72 mg, 0.51 mmol) was added slowly to the reactant at −78° C., and the mixture was stirred at room temperature for 1 hour. The reactant was cooled, diluted with water, and extracted with EtOAc. The organic layer was dried with MgSO4, filtered, and concentrated under reduced pressure. The residue was purified by column chromatography (eluent EtOAc/Hex=1/5) to obtain the title compound (60 mg, 54%).
WORKUP
后处理
- stirringthe mixture was stirred at room temperature for 1 hour
- temperatureThe reactant was cooled
- extractionextracted with EtOAc
- dry with materialThe organic layer was dried with MgSO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe residue was purified by column chromatography (eluent EtOAc/Hex=1/5)