HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 57900521, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Ethylenediamine | HCID 3301 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | HCID 57900387 | HCID 57900387 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 57900521 | HCID 57900521 | 20% |
Reaction Steps
To a solution of ethane-1,2-diamine (82 mg, 1.36 mmol) and pyridine (0.5 mL) in mL of THF was slowly added 2-(4-(2-chlorophenyl)-5-oxo-4,5-dihydro-1H-1,2,4-triazol-3-yl)-4,5-dihydrobenzo[b]thieno[2,3-d]oxepine-8-carbonyl chloride (ca. 417 mg, ca. 0.91 mmol) in mL of THF at 0° C. The mixture was stirred at room temperature overnight, diluted with water and purified by preparative HPLC to afford 66 mg of 533, isolated yield: 20%. ESI-MS: 482. 1H NMR (DMSO-d6, 400 MHz): δ 8.74 (s, 1H, NH), 8.37 (s, 1H, NH), 7.74-7.47 (m, 7H, ArH), 6.47 (s, 1H, ═CH), 4.19 (t, J=4.8 Hz, 2H, CH2), 3.40-3.36 (m, 4H, 2CH2), 2.98 (t, J=5.2 Hz, 2H, CH2), 2.86 (t, J=6.0 Hz, 2H, CH2).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08846762B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-39dc48223cb644ea986c210be4cd3065 |
| Source note | uspto-grants-2014_09 |