HRID38082

反应详情

EQUATION

反应方程式

HRID 38082 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 1-(3-methoxy-phenyl)-2-pyridin-4-yl-ethanone (1 g, 4.40 mmol) in dry DMSO (22 mL) under nitrogen atmosphere solid potassium carbonate (1.8 g, 13.20 mmol, 3 eq) was added at room temperature, followed by carbon disulfide (0.796 mL, 13.20 mmol, 3 eq) and dibromomethane (0.926 mL, 13.20 mmol, 3 eq). The reaction mixture was stirred at room temperature for 3 hour and then poured into stirred iced water (150 mL). The yellow precipitate was filtered, washed with water and dried at 60° C. under reduced pressure for 1 hour to give 1.18 g (83%) of 2-[1,3]dithietan-2-ylidene-1-(3-methoxy-phenyl)-2-pyridin-4-yl-ethanone.

WORKUP

后处理

  1. additionpoured
  2. filtrationThe yellow precipitate was filtered
  3. washwashed with water
  4. customdried at 60° C. under reduced pressure for 1 hour