Trifluoroacetic acid → HCID 117770646, compound

To a solution of 2-(3-bromo-1H-pyrazol-1-yl)-N-tritylethanamine obtained in Step B (100 mg) and triethylsilane (38.8 μL) in dichloromethane (1.2 mL) was slowly added trifluoroacetic acid (1.2 mL) under ice-cooling. The reaction mixture was warmed to room temperature, stirred for 3 hr, and concentrated under reduced pressure. To a solution of the obtained residue and acetic anhydride (32.7 μL) in dichloromethane (2.0 mL) was added triethylamine (97.0 μL) under ice-cooling, and the mixture was stirred for 2 hr. To the reaction mixture was added dichloromethane, and the mixture was washed with water and saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate) to give the title compound (40.0 mg).

1. temperaturecooling
2. concentrationconcentrated under reduced pressure
3. additionTo a solution of the obtained residue and acetic anhydride (32.7 μL) in dichloromethane (2.0 mL) was added triethylamine (97.0 μL) under ice-
4. temperaturecooling
5. stirringthe mixture was stirred for 2 hr
6. additionTo the reaction mixture was added dichloromethane
7. washthe mixture was washed with water and saturated brine
8. dry with materialdried over anhydrous sodium sulfate
9. customthe solvent was evaporated under reduced pressure
10. customThe residue was purified by silica gel column chromatography (ethyl acetate)

ORD record

ord-49386001f0894eb4a1cbcce62ef9f6d0

Source dataset

uspto-grants-2015_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09085578B2