HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 4-{Amino-[6-oxo-2-(3-trifluoromethyl-phenylamino)-cyclohex-1-enyl]-methyl}-3-methylsulfanyl-benzonitrile hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | {(4-Cyano-2-methylsulfanyl-phenyl)-[6-oxo-2-(3-trifluoromethyl-phenylamino)cyclohex-1-enyl]-methyl}-carbamic acid tert-butyl ester | HCID 118692901 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 4-{Amino-[6-oxo-2-(3-trifluoromethyl-phenylamino)-cyclohex-1-enyl]-methyl}-3-methylsulfanyl-benzonitrile hydrochloride | HCID 118692890 | — |
Reaction Steps
A solution of hydrogen chloride in 1,4-dioxane (4 M, 4.5 mL, 18 mmol) is added to a mixture of {(4-cyano-2-methylsulfanyl-phenyl)-[6-oxo-2-(3-trifluoromethyl-phenylamino)cyclohex-1-enyl]-methyl}-carbamic acid tert-butyl ester (INTERMEDIATE 4, 2.16 g, 3.25 mmol) in acetonitrile (4.5 mL) and the mixture is stirred at room temperature for 1 h. The precipitate is filtered off, washed with acetonitrile and dried. Yield: 1.19 g. ESI mass spectrum: [M+H-NH3]+=415; Retention time HPLC: 0.88 min (Z018_S04).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09440930B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-a45e5ae647e149fa90c6db25ec98a17d |
| Source note | uspto-grants-2016_09 |