反应详情

温度

75 °C

To a suspension of 1.49 g (20.6 mmol) of hydroxylamine hydrochloride in DMSO (10 mL) was added 2.88 mL (20.6 mmol) of triethylamine. The slurry was stirred for 5 min and then filtered twice through cotton, rinsing with THF, to remove the solids. The filtrate was partially concentrated under reduced pressure to remove THF, and then was added to a flask containing 915 mg (2.06 mmol) of 2-((3R,5R,6S)-5-(3-chlorophenyl)-6-(4-chlorophenyl)-3-methyl-2-oxo-1-(pentan-3-yl)piperidin-3-yl)acetonitrile (Example 82, Step B). The resulting yellow solution was heated at 75° C. for 22 h, and then was partitioned between water and EtOAc. The organic layer was dried over Na2SO4, filtered and the filtrate was concentrated. Purification of the residue by flash chromatography on silica gel (1 to 7% MeOH/DCM, gradient elution) provided the title compound as a white solid.

1. filtrationfiltered twice through cotton
2. washrinsing with THF
3. customto remove the solids
4. concentrationThe filtrate was partially concentrated under reduced pressure
5. customto remove THF
6. additionwas added to a flask
7. customwas partitioned between water and EtOAc
8. dry with materialThe organic layer was dried over Na2SO4
9. filtrationfiltered
10. concentrationthe filtrate was concentrated
11. customPurification of the residue by flash chromatography on silica gel (1 to 7% MeOH/DCM, gradient elution)