Imidazole → 3-(t-Butyldiphenylsiloxy)-3-(4-pyridyl)propionitrile

Next, imidazole (4.60 g, 67.5 mmol) and N,N-dimethylformamide (30 ml) were added to the obtained 3-hydroxy-3-(4-pyridyl)propionitrile (1.00 g, 6.75 mmol), and the mixture was stirred at room temperature. t-Butyldiphenylchlorosilane (2.23 g, 8.10 mmol) was added to the mixture, and the whole was stirred for one day and further stirred at an external temperature of 50° C. for three hours. Ethyl acetate (50 ml) and ether (50 ml) were added to the reaction mixture, the whole was washed with water (20 ml) three times and saturated brine (30 ml) successively, and the organic layer was dried over anhydrous magnesium sulfate. The organic layer was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography to give 2.58 g (98.9%) of 3-(t-butyldiphenylsiloxy)-3-(4-pyridyl)propionitrile as a colorless oily matter.

1. stirringthe whole was stirred for one day
2. stirringfurther stirred at an external temperature of 50° C. for three hours
3. washthe whole was washed with water (20 ml) three times and saturated brine (30 ml) successively
4. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
5. concentrationThe organic layer was concentrated under reduced pressure
6. customthe residue was purified by silica gel column chromatography

ORD-Eintrag

ord-5796659c7f674d9aaacb6e64badd6d98

Quelldatensatz

uspto-grants-2006_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07098226B2