HRID1525242

反应详情

EQUATION

反应方程式

HRID 1525242 的结构方程式

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of compound 2-(4-Bromophenyl)-2-phenylacetic acid, 14-c, (5.6 g, 19.3 mmol) in methanol (200 mL) was added concentrated sulfuric acid (6 mL) and the reaction mixture was stirred at 60° C. for 14 h. The resulting solution was concentrated and ice-water was added. The aqueous layer was extracted by EA. The combined organic layers were washed with brine, dried over sodium sulfate and concentrated to yield title compound, 14-d, (5.5 g, 93%). 1H NMR (300 MHz, CDCl3) δ3.73 (s, 3H), 4.96 (s, 1H), 7.16 (d, J=8.4 Hz, 2H), 7.25-7.30 (m, 5H), 7.42 (d, J=8.4 Hz, 2H). LC-MS: (M+H)+ 304, 306.

WORKUP

后处理

  1. concentrationThe resulting solution was concentrated
  2. additionice-water was added
  3. extractionThe aqueous layer was extracted by EA
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated