反应 #1905

反应方程式

sodium cyanoborohydride

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

pivalaldehyde

acetic acid

→

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

溶剂

ethanol

反应条件

后处理

1. 1
   workup.STIRRINGthe mixture was stirred for 24 h
2. 2
   浓缩After the mixture was concentrated in vacuo
3. 3
   workup.ADDITIONthe residue was diluted with water (200 ml)
4. 4
   萃取extracted with ethyl acetate (200 ml)
5. 5
   洗涤The extract was washed with water
6. 6
   干燥dried over magnesium sulfate
7. 7
   浓缩concentrated in vacuo
8. 8
   其他The residue was purified by silica gel column chromatography (hexane:ethyl acetate=5:1)

实验过程

A mixture of 2-amino-α-(4-benzyloxy-2-methoxyphenyl)-5-chlorobenzyl alcohol (9.5 g), pivalaldehyde (3.35 ml), acetic acid (1.85 g) and ethanol (200 ml) was stirred for 30 min. To the mixture was added sodium cyanoborohydride (2.33 g) and the mixture was stirred for 24 h. After the mixture was concentrated in vacuo, the residue was diluted with water (200 ml) and extracted with ethyl acetate (200 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=5:1) to give α-(4-benzyloxy-2-methoxyphenyl)-2-neopentylamino-5-chlorobenzyl alcohol (10.0 g) as a colorless oil.

来源