HRID62831

反应详情

EQUATION

反应方程式

HRID 62831 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe solution was cooled to 0˜5° C
  2. waitat room temperature for 2 hours
  3. additionwas added
  4. stirringthe mixture was stirred for 30 minutes
  5. customwas removed
  6. dry with materialThe organic layer was dried with MgSO4
  7. filtrationfiltrated
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by column chromatography (eluent, EtOAc/Hex=1/3)