反应 #1893

反应方程式

2-amino-5-chloro-2'-methoxybenzophenone

sodium bicarbonate

→

2-amino-5-chloro-2'-hydroxybenzophenone

收率 93.4%

溶剂

hydrogen bromide

反应条件

后处理

1. 1
   温度was heated for 1 hour
2. 2
   温度under reflux
3. 3
   萃取subjected to extraction with 100 ml of ethyl acetate
4. 4
   洗涤The extract solution was washed with water
5. 5
   干燥dried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONthe solvent was then distilled off under reduced pressure
7. 7
   其他The residue was purified by means of silica gel column chromatography (eluent, hexane:ethyl acetate=10:1)

实验过程

A mixture of 2.15 g of 2-amino-5-chloro-2'-methoxybenzophenone and 20 ml of 47% hydrogen bromide was heated for 1 hour under reflux. The solution was rendered neutral with sodium bicarbonate, and subjected to extraction with 100 ml of ethyl acetate. The extract solution was washed with water and dried over anhydrous magnesium sulfate; the solvent was then distilled off under reduced pressure. The residue was purified by means of silica gel column chromatography (eluent, hexane:ethyl acetate=10:1) to yield 1.9 g of 2-amino-5-chloro-2'-hydroxybenzophenone as needles, m.p. 51° to 52° C.

来源