HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxylamine → HCID 58121147, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxylamine | HCID 787 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 12477826 | HCID 12477826 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 58121147 | HCID 58121147 | 21% |
Reaction Steps
To a stirring solution of ethyl 2,5-diphenylthiophene-3-carboxylate 70 (0.440 g, 1.427 mmol) in methanol (7 mL) and THF (7 mL) was added 50% hydroxylamine in water (1.4 mL, 23.31 mmol) and the resulting mixture was stirred at room temperature for 45 minutes then concentrated to one third volume. The solution was neutralized with 3N HCl to pH 7 and the desired product was filtered then purified by Gilson (55 to 95% MeOH in H2O) to afford the title compound 71 (87 mg, 21% yield) as a white solid. 1H NMR: (DMSO-d6) d(ppm) 1H, 10.96 (s, 1H), 9.14 (s, 1H), 7.71-7.69 (m, 2H), 7.57-7.55 (m, 3H), 7.48-7.34 (m, 6H) LRMS (ESI): (calc) 295.36 (found) 296.22 (MH)+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08673911B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-15c900612c5e4e5c916c9c6eaf533f2a |
| Source note | uspto-grants-2014_03 |