反応 #1895

反応方程式

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

potassium carbonate

benzyl bromide

→

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

溶媒

N,N-dimethylformamide

反応条件

後処理

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

実験手順

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.

出典