HRID368544

反应详情

EQUATION

反应方程式

HRID 368544 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-Chlorobenzenesulfonic acid 3-benzyloxyphenyl ester (3.75 g, 10 mmol), as prepared in the preceding step, Pd/C (10%) (350 mg) in tetrahydrofuran (80 mL) was hydrogenated (balloon) for 3 h. The catalyst was filtered through Celite and washed with tetrahydrofuran. The combined tetrahydrofuran solution was evaporated in vacuo and the residue was then purified by flash column chromatography (methylene chloride) to give the title compound as a colorless oil (2.75 g, 95%). 1H-NMR (300 MHz, CDCl3) δ 6.68 (m, 3 H), 7.12 (t, 1H, J=6.5 Hz), 7.37 (t, 1H, J=7.1 Hz), 7.60 (m, 2 H), 7.94 (dd, 1H, J=0.6, 4.0 Hz).

WORKUP

后处理

  1. customfor 3 h
  2. filtrationThe catalyst was filtered through Celite
  3. washwashed with tetrahydrofuran
  4. customThe combined tetrahydrofuran solution was evaporated in vacuo
  5. customthe residue was then purified by flash column chromatography (methylene chloride)