HRID35987
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- customIn a 250 mL flask equipped with a nitrogen inlet
- temperaturereflux condenser
- temperaturecooled to room temperature
- stirringstirred for an additional 16 h
- extractionthe organics were extracted
- dry with materialdried over magnesium sulfate
- customthe solvents were removed under reduced pressure
- customto yield a yellow powder
- customRecrystallization from acetone