HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → (cis)-2-amino-N-(2,2,2-trifluoroethyl)cyclohexanecarboxamide Hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | 1,4-Dioxane hydrochloride | HCID 20443148 | — |
| Reactant | Diethylether hexane | HCID 21584099 | — |
| Reactant | Tert-butyl{(cis)-2-[(2,2,2-trifluoroethyl)carbamoyl]cyclohexyl}carbamate | HCID 97027465 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | (cis)-2-amino-N-(2,2,2-trifluoroethyl)cyclohexanecarboxamide Hydrochloride | HCID 117628534 | — |
Reaction Steps
To tert-butyl {(cis)-2-[(2,2,2-trifluoroethyl)carbamoyl]cyclohexyl}carbamate, I-5a (2.55 g, 7.86 mmol) in Dioxane (10 ml) was added 4 M HCl/Dioxane (19.66 ml, 79 mmol) and the mixture allowed to stir at RT for 60 min. The reaction was concentrated in vacuo and resulting solid slurried with diethyl ether (100 mL). Re-concentration of the mixture and re-slurry of the solid with ether/hexane gave a free flowing solid. Final concentration of the mixture gave a white solid, I-5b, (2.1 gm) which was stored under nitrogen.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09096598B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-23ac0915210640fc89faf0c5e91f373e |
| Source note | uspto-grants-2015_08 |