反応 #1904

反応方程式

2-amino-4'-benzyloxy-5-chloro-2'-methoxybenzophenone

sodium borohydride

→

2-amino-α-(4-benzyloxy-2-methoxyphenyl)-5-chlorobenzyl alcohol

収率 94.5%

溶媒

methanol

反応条件

後処理

1. 1
   濃縮the mixture was concentrated in vacuo
2. 2
   workup.ADDITIONThe residue was diluted with water (200 ml)
3. 3
   抽出extracted with ethyl acetate (300 ml)
4. 4
   洗浄The extract was washed with water
5. 5
   乾燥dried over magnesium sulfate
6. 6
   濃縮concentrated in vacuo
7. 7
   その他The residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1-2:1)

実験手順

To a solution of 2-amino-4'-benzyloxy-5-chloro-2'-methoxybenzophenone (10 g) in methanol (100 ml) was added sodium borohydride (1.4 g). After being stirred for 24 h, the mixture was concentrated in vacuo. The residue was diluted with water (200 ml) and extracted with ethyl acetate (300 ml). The extract was washed with water, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1-2:1) to give 2-amino-α-(4-benzyloxy-2-methoxyphenyl)-5-chlorobenzyl alcohol (9.5 g) as colorless crystals (mp=101°-103° C.).

出典