HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 59593326, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Triethylsilane | HCID 12052 | — |
| Reactant | 4-(Trifluoromethyl)benzaldehyde | HCID 67996 | — |
| Reactant | 2-Amino-5-bromopyridine | HCID 70622 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 59593326 | HCID 59593326 | — |
Reaction Steps
Into a round bottom flask fitted with stirrer and reflux condenser was added 2-amino-5-bromopyridine (15, 1.73 mol, 300 g) and p-trifluoromethylbenzaldehyde (16, 1.723 mol, 300 g) to a solution of trifluoroacetic acid (400 mL), triethylsilane (825 mL) and acetonitrile (7500 mL). The reaction was heated to reflux overnight (24 hours). Solvents were removed and the residue was poured into aqueous K2CO3 and extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate, and concentrated. The crude compound was crystallized with diethyl ether/hexane to afford compound 17, 420 g (73.6%) as off white solid. MS (ESI) [M+H+]+=331.1 and 333.1 (1:1 ratio).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09169250B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-af2224ed715a481d9754d57e04f77484 |
| Source note | uspto-grants-2015_10 |