反应详情

In a separate flask a solution of imine INT 36 (5 g, 18.4 mmol) in THF (140 mL) was cooled in a dry ice bath under argon to −78° C. At this temperature the organozincate solution from above was added dropwise over a period of about 30 minutes. Stirring was continued for another hour before the resulting mixture was first quenched carefully with 10% ammonium chloride solution (40 mL), then water (50 mL). The reaction mixture was allowed to warm up to room temperature and was then extracted with Et2O (3×). The organic layers were washed with water and brine, dried over sodium sulfate, filtered and concentrated. The crude was purified by chromatography on silica gel (cyclohexane/EtOAc).

1. additionAt this temperature the organozincate solution from above was added dropwise over a period of about 30 minutes
2. waitwas continued for another hour before the resulting mixture
3. customwas first quenched carefully with 10% ammonium chloride solution (40 mL)
4. extractionwas then extracted with Et2O (3×)
5. washThe organic layers were washed with water and brine
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated
9. customThe crude was purified by chromatography on silica gel (cyclohexane/EtOAc)