反应详情

温度

40 °C

1-Bromo-4-fluorobenzene (1.12 g, 6.4 mmol) of was dissolved in ether (20 ml) and cooled to −78° C. nBuLi (2.56 ml, 2.5M, 6.4 mmol) was added and the reaction mixture was stirred for 1 h. (2,2-Difluoro-2-pyridin-2-ylethylidene)-[3,3-dimethyl-1(S)-(4-methyl-2,6,7-trioxabicyclo[2.2.2]oct-1-yl)butyl]amine (1.18 g, 3.2 mmol) was added and stirring was continued for 2 h while the solution was allowed to warm up to 40° C. Water (5 ml) was added and the reaction mixture was allowed to warm to room temperature. The organic layer was separated, washed with brine and was dried over MgSO4. The solvent was evaporated and the crude was purified by flash column chromatography using silica gel and 20:80 ethylacetate:hexane as an eluent to give [2,2-difluoro-1(S)-(4-fluorophenyl)-2-pyridin-2-ylethyl]-[3,3-dimethyl-1(S)-(4-methyl-2,6,7-trioxabicyclo[2.2.2]oct-1-yl)butyl]amine (265 mg).

1. additionwas added
2. additionwas added
3. temperatureto warm to room temperature
4. customThe organic layer was separated
5. washwashed with brine
6. dry with materialwas dried over MgSO4
7. customThe solvent was evaporated
8. customthe crude was purified by flash column chromatography