反应 #45781

反应方程式

hydrogen

5-methyl-7-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-2-(2-nitrophenyl)-6-phenyl-1,3-benzoxazole-4-carbonitrile

→

compound

收率 55.0%

2-(2-Aminophenyl)7-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile

收率 55.0%

溶剂

ethyl acetate

反应条件

后处理

1. 1
   其他The catalyst was removed by filtration
2. 2
   洗涤with washing with ethyl acetate
3. 3
   浓缩the filtrate was concentrated under reduced pressure
4. 4
   洗涤Elution with a mixed solvent of chloroform/methanol (99:1→96:4, v/v)

实验过程

10% Palladium-carbon (150 mg) was added to an ethyl acetate (30 ml) solution of 5-methyl-7-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-2-(2-nitrophenyl)-6-phenyl-1,3-benzoxazole-4-carbonitrile (I-211) (128 mg, 0.27 mmol), followed by stirring at the same temperature under atmospheric pressure of hydrogen for 1.5 hours. The catalyst was removed by filtration with washing with ethyl acetate, the filtrate was concentrated under reduced pressure, and the resulting residue was subjected to silica gel column chromatography. Elution with a mixed solvent of chloroform/methanol (99:1→96:4, v/v) gave the entitled compound (65 mg, 55%) as a pale yellow solid.

来源