HRID62850

反应详情

EQUATION

反应方程式

HRID 62850 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Anhydrous THF (30 mL) in dried flask was cooled to 0° C., LAH (1.14 g, 30 mmol) was added slowly thereto, and the mixture was stirred for 30 minutes. 2-Butylsulfanyl-nicotinic acid (1.27 g, 5.58 mmol) obtained in Step A which is dissolved in anhydrous THF (10 mL) was added slowly thereto, and the mixture was stirred at room temperature for 2 hours. After the termination of the reaction, water (10 mL) was added slowly thereto at 0° C., and the mixture was stirred for 30 minutes. The reactant was extracted with EtOAc, and the organic layer was separated, dried with MgSO4, and concentrated under reduced pressure to obtain the title compound (0.85 g, 77%).

WORKUP

后处理

  1. additionwas added slowly
  2. stirringthe mixture was stirred at room temperature for 2 hours
  3. additionwas added slowly
  4. stirringat 0° C., and the mixture was stirred for 30 minutes
  5. extractionThe reactant was extracted with EtOAc
  6. customthe organic layer was separated
  7. dry with materialdried with MgSO4
  8. concentrationconcentrated under reduced pressure