HRID347299

反应详情

EQUATION

反应方程式

HRID 347299 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

bii) Alternatively, to a solution of rac-2-(4-fluoro-phenyl)-cyclohexanol (7.5 g, 39 mmol) in dry DMSO (67 mL) was added triethylamine (27 mL, 190 mmol) under argon and the resulting mixture cooled to 0° C. and then a solution of sulfur trioxide pyridine complex (18.4 g, 116 mmol) in dry DMSO (98 mL) was added dropwise over 15 min. After 1 h, the mixture was diluted with water (200 mL) and the product extracted with DCM (2×100 mL). The combined organic extracts were then dried over sodium sulfate, followed by filtration and evaporation. Purification by filtration through silica gel, eluting with ethyl acetate:hexane (1:4) afforded the title compound (7.1 g, 95%) as white crystals. MS: m/e=192.1 (M).

WORKUP

后处理

  1. extractionthe product extracted with DCM (2×100 mL)
  2. dry with materialThe combined organic extracts were then dried over sodium sulfate
  3. filtrationfollowed by filtration and evaporation
  4. customPurification
  5. filtrationby filtration through silica gel
  6. washeluting with ethyl acetate:hexane (1:4)