HRID902628

反应详情

EQUATION

反应方程式

HRID 902628 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (3-{3[(2-Chloro-3-trifluoromethyl-benzyl)-diphenylethyl-amino]-propoxy}-phenyl)-acetic acid hydrochloride salt (Example 1d, 0.1 g, 0.2 mmol) in methanol (2 ml) was added concentrated sulfuric acid (2 drops). After the resulting mixture was heated to reflux for 2 h solvent was removed under vacuum. The residue was dissolved in water and neutralized to pH=7. The aqueous layer was extracted with ethyl acetate three times. The combined organic layers were washed with, brine, dried over magnesium sulfate, and concentrated in vacco to give 900 mg (93%) of the title compound as an oil. MS m/e 596.2 (M+H)+.

WORKUP

后处理

  1. temperatureAfter the resulting mixture was heated
  2. temperatureto reflux for 2 h solvent
  3. customwas removed under vacuum
  4. dissolutionThe residue was dissolved in water and neutralized to pH=7
  5. extractionThe aqueous layer was extracted with ethyl acetate three times
  6. washThe combined organic layers were washed with, brine
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated in vacco