反応 #1894

反応方程式

2-acetylamino-5-chloro-2'-methoxybenzophenone

sodium hydroxide

→

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

収率 98.1%

溶媒

hydrogen bromide

反応条件

後処理

1. 1
   温度was heated for 2 hours
2. 2
   温度under reflux
3. 3
   抽出was subjected to extraction with 200 ml of ethyl acetate
4. 4
   洗浄The extract solution was washed with water
5. 5
   乾燥dried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONthe solvent was then distilled off under reduced pressure
7. 7
   その他The residue was purified by means of silica gel column chromatography (eluent, hexane:ethyl acetate=5:1)

実験手順

A mixture of 10 g of 2-acetylamino-5-chloro-2'-methoxybenzophenone and 100 ml of 47% hydrogen bromide was heated for 2 hours under reflux. The solution was rendered neutral with sodium hydroxide, and was subjected to extraction with 200 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=5:1) to yield 8.0 g of 2-amino-5-chloro-2'-hydroxybenzophenone as needles.

出典