HRID62831
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
2-Isopropylsulfanyl-nicotinic acid obtained in Step A was dissolved in THF (50 mL), and the solution was cooled to 0˜5° C. LAH (3.06 g, 80.55 mmol) was added thereto slowly, and the mixture was stirred at 0˜5° C. for 30 minutes and then at room temperature for 2 hours. After the termination of the reaction, saturated sodium sulfate aqueous solution was added thereto and the mixture was stirred for 30 minutes. After the addition of EtOAc, solid material was removed by using cellite. The organic layer was dried with MgSO4, filtrated and concentrated under reduced pressure. The residue was purified by column chromatography (eluent, EtOAc/Hex=1/3) to obtain the title compound (3.94 g, 67%).
WORKUP
后处理
- temperaturethe solution was cooled to 0˜5° C
- waitat room temperature for 2 hours
- additionwas added
- stirringthe mixture was stirred for 30 minutes
- customwas removed
- dry with materialThe organic layer was dried with MgSO4
- filtrationfiltrated
- concentrationconcentrated under reduced pressure
- customThe residue was purified by column chromatography (eluent, EtOAc/Hex=1/3)