HRID1713794

反应详情

EQUATION

反应方程式

HRID 1713794 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

10% Pd/C (4520 mg) was added to a solution of methyl [trans-4-(4-{[(trifluoromethyl)sulfonyl]oxy}phenyl)cyclohexyl]acetate (prepared as described in Patent Application WO2004/047755) (8100 mg) in MeOH (150 mL). The resulting suspension was stirred for 16 h under an atmosphere of Hydrogen. The suspension was filtered through diatomaceous earth and concentrated in vacuo to give a slurry. This was extracted into EtOAc (300 mL). The organic extract was washed with saturated aqueous sodium hydrogen carbonate solution (75 mL) and then brine (75 mL). The organic layer was dried and concentrated in vacuo to give the title compound (4720 mg) as an oil; 1H NMR δ 7.28-7.11 (5H, m), 3.58 (3H, s), 2.43 (1H+DMSO, m), 2.22 (2H, d), 1.83-1.67 (5H, m), 1.44 (2H, m), 1.13 (2H, m); MS m/e MH+ 233.

WORKUP

后处理

  1. filtrationThe suspension was filtered through diatomaceous earth
  2. concentrationconcentrated in vacuo
  3. customto give a slurry
  4. extractionThis was extracted into EtOAc (300 mL)
  5. extractionThe organic extract
  6. washwas washed with saturated aqueous sodium hydrogen carbonate solution (75 mL)
  7. customThe organic layer was dried
  8. concentrationconcentrated in vacuo