HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Chloro-3,6-difluorophenol → 4-(2-Chloro-3,6-difluoro-phenoxy)-6-[6-(4-methylpiperazin-1-yl)-pyridin-3-yl]-1,2,3,4-tetrahydro-[1,8]naphthyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Chloro-3,6-difluorophenol | HCID 2773561 | — |
| Reactant | 6-[6-(4-Methylpiperazin-1-yl)pyridin-3-yl]-1,2,3,4-tetrahydro-[1,8]naphthyridin-4-ol | HCID 57885829 | — |
| Solvent | Dichloromethane methanol | HCID 21226129 | — |
| Product | 4-(2-Chloro-3,6-difluoro-phenoxy)-6-[6-(4-methylpiperazin-1-yl)-pyridin-3-yl]-1,2,3,4-tetrahydro-[1,8]naphthyridine | HCID 46906672 | 54% |
Reaction Steps
6-[6-(4-Methylpiperazin-1-yl)pyridin-3-yl]-1,2,3,4-tetrahydro-[1,8]naphthyridin-4-ol (85 mg) was reacted with 2-chloro-3,6-difluorophenol (50 mg) as in General Procedure 12. Silica gel chromatography using a gradient of 0-10% methanol/CH2Cl2 as the eluting solvent gave the title compound as a yellow foam (54% yield). LCMS: m/z=472 (M+H+), 1H-NMR (DMSO-d6, 400 MHz) δ 1.89 (m, 1H), 2.21 (s, 3H), 2.24 (m, 1H), 2.39 (t, J=4.8 Hz, 4H), 3.40 (m, 1H), 3.47 (t, J=4.8 Hz, 4H), 3.63 (m, 1H), 6.82 (d, J=8.8 Hz, 1H), 7.03 (d, J=2.3 Hz, 1H), 7.17 (d, J=2.3 Hz, 1H) 7.25 (m, 1H), 7.39 (m, 1H), 7.52 (dd, J=2.5, 8.8 Hz, 1H), 8.08 (d, J=2.5 Hz, 1H), 8.19 (d, J=2.5 Hz, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08080561B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-00bcef479afc4c05a546daec3fa9ec4e |
| Source note | uspto-grants-2011_12 |