HRID333036

反应详情

EQUATION

反应方程式

HRID 333036 的结构方程式

PROCEDURE

实验过程

A mixture of N-(3,4-difluorophenyl)chloroacetamide (14 mmol) and aluminum chloride (54 mmol) was stirred and heated to 200-210 deg C. in a silicon oil bath for 4.5 h. On cooling, 40 mL of ice cold hydrochloric acid was added to the reaction mixture. The solid residue was removed by vacuum filtration and purified by column chromatography with hexane-ethyl acetate (1:1) as eluting solvent. The yield for this step was 40.7%. 1HNMR (300 MHz, in DMSO-d6) δ 10.46 (s, 1H, NH), 7.33 (t, J=8.7 Hz, 1H, Ar—H), 6.82 (q, J=6.9 Hz, 1H, Ar—H), 3.47 (s, 2H, ArCH2CO).

WORKUP

后处理

  1. temperatureheated to 200-210 deg C
  2. temperatureOn cooling
  3. customThe solid residue was removed by vacuum filtration
  4. custompurified by column chromatography with hexane-ethyl acetate (1:1)
  5. washas eluting solvent
  6. customThe yield for this step