反应 #42665

反应方程式

Trifluoroacetic acid

benzyl (3R)-6-(2,3-difluorophenyl)-1-(2,4-dimethoxybenzyl)-2-oxo-2,3,4,7-tetrahydro-1H-azepin-3-ylcarbamate

→

title compound

收率 66.4%

Benzyl (3R)-6-(2,3-difluorophenyl)-2-oxo-2,3,4,7-tetrahydro-1H-azepin-3-ylcarbamate

收率 66.4%

溶剂

dichloromethane

反应条件

后处理

1. 1
   浓缩the mixture was concentrated at 25° C.
2. 2
   workup.ADDITIONmethanol (150 mL) was added
3. 3
   过滤the precipitate filtered
4. 4
   浓缩The filtrate was concentrated
5. 5
   workup.ADDITIONdiluted with dichloromethane (100 mL)
6. 6
   洗涤washed with water (2×), saturated aqueous sodium bicarbonate (2×), saturated brine
7. 7
   干燥dried over magnesium sulfate
8. 8
   过滤filtered
9. 9
   浓缩concentrated
10. 10
    其他Purification by silica gel chromatography (5% ethyl acetate/hexanes→65% ethyl acetate/hexanes)

实验过程

Trifluoroacetic acid (60 mL) was added to a solution of benzyl (3R)-6-(2,3-difluorophenyl)-1-(2,4-dimethoxybenzyl)-2-oxo-2,3,4,7-tetrahydro-1H-azepin-3-ylcarbamate (3.70 g, 7.08 mmol) in dichloromethane (40 mL). After 18 h, the mixture was concentrated at 25° C., methanol (150 mL) was added, and the precipitate filtered. The filtrate was concentrated, diluted with dichloromethane (100 mL), washed with water (2×), saturated aqueous sodium bicarbonate (2×), saturated brine, dried over magnesium sulfate, filtered and concentrated. Purification by silica gel chromatography (5% ethyl acetate/hexanes→65% ethyl acetate/hexanes) gave the title compound (1.75 g). MS 373.1 (M+1).

来源