HRID1167816

反应详情

EQUATION

反应方程式

HRID 1167816 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 2-(4-chloro-2-trifluoromethylphenyl)-ethanol in acetone (50 mL) at 0° C. was added dropwise a solution of Jones reagent (40.3 mL of a 2.67 M solution in H2SO4). After 25 min, the mixture was poured onto Et2O/H2O and the layers were separated. The organic layer was washed with H2O and brine, dried (MgSO4) and the solvent was removed in vacuo. The resultant orange solid was crystallized from hexane and heptane to furnish the title compound as a solid which showed: 1H NMR (300 MHz, CDCl3) δ 7.67 (d, 1H, J=2.0Hz), 7.51 (dd, 1H, J=2.0, 8.0Hz), 7.34 (d, 1H, J=8.0Hz), 3.84 (s, 2H).

WORKUP

后处理

  1. additionthe mixture was poured onto Et2O/H2O
  2. customthe layers were separated
  3. washThe organic layer was washed with H2O and brine
  4. dry with materialdried (MgSO4)
  5. customthe solvent was removed in vacuo
  6. customThe resultant orange solid was crystallized from hexane and heptane