反应 #1904
ord-8a08d4d95931403fb13cf9932fe3b98e
反应方程式
2-amino-4'-benzyloxy-5-chloro-2'-methoxybenzophenone
sodium borohydride
→
2-amino-α-(4-benzyloxy-2-methoxyphenyl)-5-chlorobenzyl alcohol
收率 94.5%
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1浓缩the mixture was concentrated in vacuo
- 2workup.ADDITIONThe residue was diluted with water (200 ml)
- 3萃取extracted with ethyl acetate (300 ml)
- 4洗涤The extract was washed with water
- 5干燥dried over magnesium sulfate
- 6浓缩concentrated in vacuo
- 7其他The residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1-2:1)
实验过程
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.).