HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 68070459, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 86706474 | HCID 86706474 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68070459 | HCID 68070459 | 51% |
Reaction Steps
A similar procedure was used as describe for the synthesis of 2-(3,5-dichlorophenylamino)-1-(3-(7H-pyrrolo[2,3-d]pyrimidin-4-ylamino) azepan-1-yl) ethanone to afford a residue which was subjected to column chromatography (silica gel, gradient MeOH in CH2Cl2) to afford (45 mg, 51%) the titled compound. 1H NMR (DMSO-d6, 400 MHz): 11.50 and 11.40 (2s, 1H), 8.18-8.10 (2s, 1H), 7.18 (bs, 1H), 7.08 (bs, 1H), 6.66 and 6.60 (2s, 2H), 6.58 and 6.50 (2s, 1H), 6.21 and 6.08 (2s, 2H), 4.62 and 4.46 (2s, 1H), 3.88-3.48 (m, 2H), 3.10-2.90 (m, 2H), 2.72-2.50 (m, 1H), 2.24-2.10 (m, 2H), 1.82-1.62 (m, 3H). LC-MS: m/z [M+1]=431.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09273028B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-14c6caac1866418aa409f13b761e881c |
| Source note | uspto-grants-2016_03 |