HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → HCID 90017290, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | HCID 90018297 | HCID 90018297 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 90017290 | HCID 90017290 | 82.9% |
Reaction Steps
Bromine (1.7 g, 548 μl, 10.6 mmol, Eq: 5) was added to 6-methyl-3-(trifluoromethyl)pyridin-2-amine (375 mg, 2.13 mmol, Eq: 1) in trifluoroacetic acid (7 ml). The mixture was stirred for 30 min and then concentrated to an oil. Water (30 ml) and dichloromethane (10 ml) were added. The mixture was alkalized by addition of sodium bicarbonate and extracted with dichloromethane. The combined organic layers were dried over sodium sulfate and concentrated to an oil. The crude product was purified by chromatography (SiO2, ethyl acetate/n-heptane) to give the desired product (450 mg, 82.9%) as a yellow solid. MS: m/z=255.1 (M+H+)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09394311B2 |
| Source dataset | uspto-grants-2016_07 |
| ORD ID | ord-4e24e0f5ee1d4c4f95ae198632bf243f |
| Source note | uspto-grants-2016_07 |