HRID976037

反应详情

EQUATION

反应方程式

HRID 976037 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

2-Chlorobenzoyl chloride (1.27 ml), tri-n-butyl-((3,5-bis(trifluoromethyl)phenyl)methyloxymethyl)tin (part (a), 6.2 g) and benzylchlorobis(triphenylphosphine)palladium (II) (80 mg) were dissolved in chloroform (10 ml) and the solution heated to 70° C. for 36 hours. On cooling diethyl ether and saturated aqueous potassium fluoride were added and this solution filtered through a pad of Hyflo. The organic layer was washed with water, dried (MgSO4) and reduced in vacuo giving a residue which was purified by chromatography on silica gel to give 2'-chloro-2-((3,5-bis(trifluoromethyl)phenyl) methyloxy)acetophenone, 1H NMR (360MHz, CDCl3) δ 7.79 (3H, bs, bis(CF3) aryl CH2,4,6), 7.54-7.26 (4H, m, aryl), 4.75 (2H, s), 4.76 (2H, s).

WORKUP

后处理

  1. additionwere added
  2. filtrationthis solution filtered through a pad of Hyflo
  3. washThe organic layer was washed with water
  4. dry with materialdried (MgSO4)
  5. customgiving a residue which
  6. customwas purified by chromatography on silica gel