반응 #1895

반응 방정식

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

potassium carbonate

benzyl bromide

→

2-amino-2'-benzyloxy-5-chlorobenzophenone

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   추출The mixture was subjected to extraction with 150 ml of water and 200 ml of ethyl acetate
2. 2
   세척the ethyl acetate layer was washed with water
3. 3
   건조dried over anhydrous magnesium sulfate
4. 4
   workup.DISTILLATIONdistilled off under reduced pressure
5. 5
   기타The residue was purified by means of silica gel column chromatography (eluent, hexane:ethyl acetate=10:1 to 5:1)

실험 절차

In 30 ml of N,N-dimethylformamide was dissolved 5.0 g of 2-amino-5-chloro-2'-hydroxybenzophenone, as obtained in Example 123 (1), to which were added 4.2 g of potassium carbonate and 2.9 ml of benzyl bromide; the mixture was then stirred for 2 hours at room temperature. The mixture was subjected to extraction with 150 ml of water and 200 ml of ethyl acetate, and the ethyl acetate layer was washed with water, dried over anhydrous magnesium sulfate, and distilled off under reduced pressure. The residue was purified by means of silica gel column chromatography (eluent, hexane:ethyl acetate=10:1 to 5:1) to yield 6.4 g of 2-amino-2'-benzyloxy-5-chlorobenzophenone as prism crystals, m.p. 110° to 111° C.

출처