HRID1846032

反应详情

EQUATION

反应方程式

HRID 1846032 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Bromo-2-(difluoromethyl)-4-fluorobenzene (Preparation 50, 772 mg, 3.43 mmol) and sodium ethanethiolate (352.7 mg, 3.77 mmol) in DMSO (5 mL) was heated at 50° C. for 18 hours. On cooling, water (70 mL) was added to the reaction mixture, the product was extracted with EtOAc (20 mL×3). The combined organic layers were concentrated to give the crude product, which was purified by silica gel column chromatography eluting with heptane to afford the title compound as a colourless oil (260 mg, 28%).

WORKUP

后处理

  1. temperatureOn cooling
  2. extractionthe product was extracted with EtOAc (20 mL×3)
  3. concentrationThe combined organic layers were concentrated
  4. customto give the crude product, which
  5. customwas purified by silica gel column chromatography
  6. washeluting with heptane