HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → (4-Chloro-benzyl)-(6-chloro-pyridin-2-yl)-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | 4-Chlorobenzaldehyde | HCID 7726 | — |
| Reactant | Triethylsilane | HCID 12052 | — |
| Reactant | (5-Bromo-6-fluoro-pyridin-2-yl)-(4-chloro-benzyl)-amine | HCID 57619198 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | (4-Chloro-benzyl)-(6-chloro-pyridin-2-yl)-amine | HCID 57619237 | — |
Reaction Steps
To 6-chloro-pyridin-2-ylamine (537, 5.60 g, 0.0436 mol) in acetonitrile (300 mL) were added 4-chlorobenzaldehyde (40, 6.7 g, 0.048 mol), trifluoroacetic acid (13 mL, 0.17 mol) and triethylsilane (21 mL, 0.13 mol). The reaction was heated to reflux for 4 hours, then concentrated, poured into water, extracted with ethyl acetate, and washed with sodium bicarbonate and brine. The organic layer was dried over anhydrous sodium sulfate, filtered and concentrated. The filtrate was purified with silica gel column chromatography eluting with 20% to 100% ethyl acetate in hexane to give a white solid (538, 6.5 g, 59%). MS (ESI) [M+H+]+=255.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09169250B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-d10c52c06a5140548e5114c7aff14bc1 |
| Source note | uspto-grants-2015_10 |