HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 86681562, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | tert-Butyl 2-((2,2,2-trifluoroethyl)carbamoyl)hydrazinecarboxylate | HCID 86722559 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 86681562 | HCID 86681562 | 109% |
Reaction Steps
To a stirred solution of tert-butyl 2-((2,2,2-trifluoroethyl)carbamoyl)hydrazinecarboxylate (1.62 g, 6.30 mmol) in anhydrous dioxane (10.0 mL) was added HCl (4M in dioxane, 2-3 mL). The reaction mixture was stirred at ambient temperature for 18 h, then heated at reflux for 2-3 h. The reaction mixture was allowed to cool to ambient temperature and then evaporated to afford the title compound as a white solid (1.33 g, 109%): 1H NMR (400 MHz, DMSO-d6) δ 10.12 (s, 3H), 9.25 (s, 1H), 7.72 (t, J=6.5 Hz, 1H), 3.91 (qd, J=9.7, 6.5 Hz, 2H); 19F NMR (376 MHz, DMSO-d6) δ −71.41; ESIMS m/z 156 ([M−H]−). This material is used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09215870B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-66cc13653bcf4cbaae4c2ce736648448 |
| Source note | uspto-grants-2015_12 |