Trityl chloride → 6-chloro-3-(4-fluorophenyl)-1-trityl-1H-pyrazolo[4,3-c]pyridine

Temperatur

0 °C

6-Chloro-3-(4-fluorophenyl)-1H-pyrazolo[4,3-c]pyridine (1 g, 4.04 mmol) was dissolved in DMF (20 mL) and cooled to 0° C. Sodium hydride (0.242 g, 6.06 mmol) was then added and the reaction mixture stirred for one hour. Trityl chloride (1.351 g, 4.85 mmol) was then added and the reaction mixture warmed to room temperature and stirred for 1.5 hours. The reaction mixture was diluted with water and stirred at 0° C. for one hour to promote perception. The solid was filtered and rinsed with water. The solid was diluted with DCM and concentrated in vacuo while loading onto silica gel. The residue was purified by flash chromatography (2-30% EtOAc/isohexane) to give 6-chloro-3-(4-fluorophenyl)-1-trityl-1H-pyrazolo[4,3-c]pyridine (1.63 g, 3.33 mmol, 82%). MS ESI calc'd. For C31H21ClFN3 [M+1]+ 490, found 490.

1. temperaturethe reaction mixture warmed to room temperature
2. stirringstirred for 1.5 hours
3. stirringstirred at 0° C. for one hour
4. filtrationThe solid was filtered
5. washrinsed with water
6. additionThe solid was diluted with DCM
7. concentrationconcentrated in vacuo
8. customThe residue was purified by flash chromatography (2-30% EtOAc/isohexane)

ORD-Eintrag

ord-d2a6f09b87d14c51a78e53043bce8278

Quelldatensatz

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09023865B2