HRID35987

反应详情

EQUATION

反应方程式

HRID 35987 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

In a 250 mL flask equipped with a nitrogen inlet, overhead stirring assembly, and reflux condenser were placed 3-nitrobenzoyl chloride (28 g, 0.15 mol), bromobenzene (130 g, 0.83 mol), and aluminum chloride (22 g, 0.16 mol). The mixture was heated for 3 h at 100° C., then cooled to room temperature and stirred for an additional 16 h. The mixture was poured into 1 L of acidic (HCl) ice water, and the organics were extracted using methylene chloride, dried over magnesium sulfate, and the solvents were removed under reduced pressure to yield a yellow powder. Recrystallization from acetone afforded 42.1 g (90% yield) of white crystals: m.p. 104°-105° C.

WORKUP

后处理

  1. customIn a 250 mL flask equipped with a nitrogen inlet
  2. temperaturereflux condenser
  3. temperaturecooled to room temperature
  4. stirringstirred for an additional 16 h
  5. extractionthe organics were extracted
  6. dry with materialdried over magnesium sulfate
  7. customthe solvents were removed under reduced pressure
  8. customto yield a yellow powder
  9. customRecrystallization from acetone