HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 178486132, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | N,N-dimethyl-4-{2-[2-(7-thioxo-azepan-2-yl)-ethyl]-3H-imidazo[4,5-b]pyridin-6-yl}-benzenesulfonamide | HCID 178486134 | — |
| Reactant | HCID 178508386 | HCID 178508386 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178486132 | HCID 178486132 | — |
Reaction Steps
The title compound is synthesized as described for 7-[2-(6-phenyl-3H-imidazo[4,5-b]pyridin-2-yl)-ethyl]-4,5,6,7-tetrahydro-3H-azepin-2-ylamine (compound 1) from 50 mg of N,N-dimethyl-4-{2-[2-(7-thioxo-azepan-2-yl)-ethyl]-3H-imidazo[4,5-b]pyridin-6-yl}-benzenesulfonamide (compound A5) and 2.53 ml of methanol containing ammonia (strength: 7.0 M) at 50° C. for 65 hours. Purification by flash chromatography on LiChroprep-NH2® (eluent: dichloromethane/0-10 vol. % methanol) and lyophilisation from dioxane/water (10:1 parts by volume) afford 32 mg of the title compound as an amorphous, colorless solid of m.p. 195° C. (decomp.). ESI-MS: 441.2 (MH+). TLC: Rf=0.44 (LiChroprep-NH2® HPTLC, methanol/water 10:1 parts by volume).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07790710B2 |
| Source dataset | uspto-grants-2010_09 |
| ORD ID | ord-e8ba4f6bc32249179f5dd56742bf431a |
| Source note | uspto-grants-2010_09 |