HRID924650

反应详情

EQUATION

反应方程式

HRID 924650 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of ethyl 2-(thiophen-3-yl)acetate (2.3 g, 16.2 mmol) in anhydrous THF (20 mL) was added LiHMDS (19.4 mL, 19.44 mmol) at −78° C. After stirring at that temperature for 0.5 h, a solution of nicotinoyl chloride (2.8 g, 16.2 mmol) in anhydrous THF (10 mL) was added into the reaction mixture and stirred at −78° C. for 4 hours. The mixture was quenched with NH4Cl solution, extracted with EtOAc. The organic layer was concentrated in vacuo and purified by silica gel column chromatography (1.7 g, yield 38%).

WORKUP

后处理

  1. stirringstirred at −78° C. for 4 hours
  2. customThe mixture was quenched with NH4Cl solution
  3. extractionextracted with EtOAc
  4. concentrationThe organic layer was concentrated in vacuo
  5. custompurified by silica gel column chromatography (1.7 g, yield 38%)