HuagongsheHuagongshe Chemistry Print Report · For research reference only
8-Amino-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one → HCID 66829999, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 8-Amino-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one | HCID 4615168 | — |
| Reactant | 2-(2,5-Dichloropyrimidin-4-ylamino)-N-methylbenzamide | HCID 57974132 | — |
| Product | HCID 66829999 | HCID 66829999 | 18% |
Reaction Steps
Following the procedure of 512f, 8-amino-1,3,4,5-tetrahydro-benzo[b]azepin-2-one (0.091 g, 0.0005 mol) and 2-(2,5-dichloro-pyrimidin-4-ylamino)-N-methyl benzamide (0.1 g, 0.00033 mol) were reacted. Purification by ISCO chromatography gave 2-[5-Chloro-2-(2-oxo-2,3,4,5-tetrahydro-1H-benzo[b]azepin-8-ylamino)-pyrimidin-4-ylamino]-N-methyl benzamide (0.026 g, 18%) as a tan solid. MP: 293-5° C.; 1H-NMR (DMSO-d6) δ 11.63 (s, 1H), 9.45 (d, 2H), 8.74 (s, 2H), 8.22 (s, 1H), 7.74 (d, 1H), 7.43-7 (t, 1H), 7.37-9 (d, 1H), 7.34 (s, 1H), 7.12-3 (d, 2H), 4.12 (m, 1H), 3.50 (m, 1H), 3.25 (s, 1H), 2.80-1 (d, 9H), 2.61-4 (m, 2H); LC/MS (ESI+): 437 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08552186B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-88c4f36692874cfbaa07a29cf32600de |
| Source note | uspto-grants-2013_10 |