HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,4-Difluorobenzylamine → HCID 22050838, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,4-Difluorobenzylamine | HCID 2733244 | — |
| Reactant | HCID 54724198 | HCID 54724198 | — |
| Product | HCID 22050838 | HCID 22050838 | — |
Reaction Steps
1-(2,6-difluorophenyl)-4-hydroxy-6-methylpyridin-2(1H)-one (0.3 g, 1.26 mmol) and 2,4-difluoro benzylamine (1 mL, 8.4 mmol) were combined in a nitrogen flushed culture tube. The tube was capped and heated at 180 C for 24 h. The excess amine was distilled in vacuo and the residue was chromatographed on silica (1:1 hexanes:ethyl acetate). The compound was approximately 50% pure and was carried on without further purification (0.633 g). 1H NMR (400 MHz, CD3OD) δ 7.53 (m, 1H), 7.41 (m, 1H), 7.16 (t, J=8.8 Hz, 2H), 6.93 (m, 2H), 6.00 (s, 1H), 5.42 (s, 1H), 5.42 (s, 1H), 4.37 (s, 2H), 1.93 (s, 3H) ppm. LC/MS, tr=4.65 minutes (5 to 95% acetonitrile/water over 8 minutes at 1 ml/min with detection 254 nm, at 50° C.). ES-MS m/z 363 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07629363B2 |
| Source dataset | uspto-grants-2009_12 |
| ORD ID | ord-74df5c6cb87e4a6fb4648d724f2c0ce6 |
| Source note | uspto-grants-2009_12 |