反应详情

To a solution of 1,2-difluoro-3-nitrobenzene from Example B1 (1.9 g, 12 mmol) in acetonitrile (75 ml) were added glycine ethyl ester hydrochloride (1.7 g, 12 mmol), potassium fluoride (1.2 g, 20 mmol), 18-crown-6 (309 mg, 1.2 mmol) and diisopropylethylamine (4.6 ml, 26 mmol). The mixture was stirred at reflux for 3 h, cooled and evaporated in vacuo. The residue was partitioned between water and EtOAc. The organic layer was washed with brine, filtered and evaporated in vacuo. The residue was purified by flash chromatography on silica (eluant EtOAc:pet. ether 20:80); yield 2.1 g, 73%.

1. temperatureat reflux for 3 h
2. temperaturecooled
3. customevaporated in vacuo
4. customThe residue was partitioned between water and EtOAc
5. washThe organic layer was washed with brine
6. filtrationfiltered
7. customevaporated in vacuo
8. customThe residue was purified by flash chromatography on silica (eluant EtOAc:pet. ether 20:80)