반응 #1893

반응 방정식

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

sodium bicarbonate

→

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

수율 93.4%

용매

hydrogen bromide

반응 조건

후처리

1. 1
   온도was heated for 1 hour
2. 2
   온도under reflux
3. 3
   추출subjected to extraction with 100 ml of ethyl acetate
4. 4
   세척The extract solution was washed with water
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONthe solvent was then distilled off under reduced pressure
7. 7
   기타The residue was purified by means of silica gel column chromatography (eluent, hexane:ethyl acetate=10:1)

실험 절차

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.

출처