1,1,1-Trifluoro-2-methylpropan-2-ol → Pyridin-2-yl 1,1,1-trifluoro-2-methylpropan-2-yl carbonate

Temperature

0 °C

To a slurry of KH (1.03 g, 25.8 mmol) in THF (70 mL) was added 1,1,1-trifluoro-2-methylpropan-2-ol (3 g, 23.42 mmol). The reaction was stirred at 0° C. for 20 min. A solution of dipyridin-2-yl carbonate (5.06 g, 23.42 mmol) in THF (30 mL) was then added to the mixture. The mixture was stirred at rt for overnight. A lot of solid came out from the solution. The solid was filtered and washed with EtOAc (30 mL). The combined THF/EtOAc solution was washed with water. The organic layer was dried over Na2SO4, filtered and concentrated. The obtained white solid (1.24 g, 21%) was directly used for the next step.

1. stirringThe mixture was stirred at rt for overnight
2. filtrationThe solid was filtered
3. washwashed with EtOAc (30 mL)
4. washThe combined THF/EtOAc solution was washed with water
5. dry with materialThe organic layer was dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated

ORD record

ord-e99591a7cc014056988432b59e065cf1

Source dataset

uspto-grants-2011_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07888464B2