HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 68070445, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 56968328 | HCID 56968328 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68070445 | HCID 68070445 | 23% |
Reaction Steps
A similar procedure was used as describe for the synthesis of 2-(3,5-dichloro-phenylamino)-1-{3-[methyl-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-amino]-azepan-1-yl}-ethanone to give a residue that was subjected to column chromatography (silica gel, gradient MeOH in CH2Cl2) to afford (10 mg, 23%) the titled compound. 1H NMR (DMSO-d6, 400 MHz): 11.88 (bs, 1H), 8.18 (s, 1H), 7.22 (d, J=4.0 Hz, 1H), 6.66 (s, 2H), 6.60 (s, 1H), 6.50-6.22 (m, 1H), 5.58-5.42 (m, 1H), 4.54 (t, J=8.0 Hz, 2H), 4.40-4.28 (m, 1H), 4.24 (t, J=8.0 Hz, 1H), 4.16-4.08 (m, 1H), 3.36 (s, 3H) 3.80 (d, J=2.0 Hz, 1H). LC-MS: m/z [M+1]=405.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09273028B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-a83d41baa9ac45a8a434cab7f240bb80 |
| Source note | uspto-grants-2016_03 |