HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 69939587, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 59050115 | HCID 59050115 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 69939587 | HCID 69939587 | — |
Reaction Steps
The compound of Example 9 (1369,8 mg, 2.07 mmol, 1 equiv) was dissolved in dioxane (4 mL) and treated with a 1M solution of hydrochloric acid in dioxane (4.5 mL, 4.5 mmol, 2.2 equiv) at room temperature. The reaction mixture was stirred for 3.5 h at ambient temperature. The solvents were removed under reduced pressure and the crude product was titurated with diethylether. The white precipitate was filtered off and dried in vacuuo. Yield 615.4 mg, 65.2% of a white solid. 1H NMR (DMSO, 200 MHz) δ 9.69 (s, 1H-NH); 8.95 (s, 2H); 8.79 (d, 1H); 8.52-8.38 (m, 1H); 7.99-7.72 (m, 3H); 7.55-7.32 (m, 4H); 7.25-7.17 (m, 3H); 7.02 (d, 1H); 4.82-4.59 (m, 2H); 4.51-4.40 (m, 1H); 3.80 (s, 3H), 2.55 (s, 2H). MS (ESI) 443 (M+Na), 421 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06545029B2 |
| Source dataset | uspto-grants-2003_04 |
| ORD ID | ord-f05af4375f134a14b75891935c130940 |
| Source note | uspto-grants-2003_04 |