反应 #1868

反应方程式

water

2-amino-5-chloro-α-(2-chloro phenyl)benzyl alcohol

2,4-dimethoxy benzaldehyde

sodium borohydride

→

5-chloro-α-(2-chlorophenyl)-2-(2,4-dimethoxybenzyl)aminobenzyl alcohol

收率 96.1%

溶剂

acetic acid

反应条件

后处理

1. 1
   温度cooling
2. 2
   萃取followed by extraction with ethyl acetate (200 ml×2)
3. 3
   洗涤The ethyl acetate layer was washed with 1N sodium hydroxide, which
4. 4
   干燥was dried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONby distilling off the solvent under reduced pressure
6. 6
   其他The residue was purified by means of a silica gel column chromatography (hexane:ethyl acetate=5:1)

实验过程

To a solution of 2-amino-5-chloro-α-(2-chloro phenyl)benzyl alcohol (5.0 g) and 2,4-dimethoxy benzaldehyde (3.72 g) in acetic acid (50 ml) was added, under ice-cooling, sodium borohydride (0.94 g). The mixture was stirred for one hour at room temperature, which was poured into water (200 ml), followed by extraction with ethyl acetate (200 ml×2). The ethyl acetate layer was washed with 1N sodium hydroxide, which was dried over anhydrous magnesium sulfate, followed by distilling off the solvent under reduced pressure. The residue was purified by means of a silica gel column chromatography (hexane:ethyl acetate=5:1) to give 5-chloro-α-(2-chlorophenyl)-2-(2,4-dimethoxybenzyl)aminobenzyl alcohol (7.5 g) as an oily product.

来源