HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 71529262, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | HCID 86689159 | HCID 86689159 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 71529262 | HCID 71529262 | 65.9% |
Reaction Steps
3-Chloro-5-trifluoromethyl-pyridine-2-carboxylic acid [6-((R)-5,5-difluoro-2-{[(4-methoxy-phenyl)-(3-methoxy-phenyl)-phenyl-methyl]-amino}-4-methyl-5,6-dihydro-4H-[1,3]oxazin-4-yl)-5-fluoro-pyridin-2-yl]-amide (80 mg, 0.104 mmol) was dissolved in dichloromethane (0.1039 ml), TFA (80.0 μl, 1.04 mmol) was added and the reaction mixture was stirred at rt for 18 hours. The reaction mixture was poured onto a mixture of ice ethyl acetate and NH4OH (w=25%). The organic layer was washed with water, brine, dried over sodium sulfate, filtered and concentrated. The crude product was chromatographed over silica gel (column 4 g, dichloromethane/methanol 95:5+0.5% ammonia) to give the title compound: 32 mg (65.9% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09163011B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-e7fa1528823547b286de36cfb1b7e362 |
| Source note | uspto-grants-2015_10 |