HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 118692142, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | {(2-Bromo-4-cyano-phenyl)-[6-oxo-2-(3-trifluoromethyl-phenylamino)-cyclohex-1-enyl]-methyl}-carbamic acid tert-butyl ester | HCID 118692170 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 118692142 | HCID 118692142 | — |
Reaction Steps
{(2-Bromo-4-cyano-phenyl)-[6-oxo-2-(3-trifluoromethyl-phenylamino)-cyclohex-1-enyl]-methyl}-carbamic acid tert-butyl ester (INTERMEDIATE 20, 20.8 g, 36.9 mmol) is suspended in acetonitrile (150 mL) and a solution of hydrogen chloride in 1,4-dioxane (4 M, 46.1 mL, 184.3 mmol) is added. The mixture is stirred at room temperature for 3 h. The product precipitates from the reaction mixture. The precipitate is filtered off, washed with acetonitrile and dried. Yield: 16.5 g ESI mass spectrum: [M+H]+=464 (bromine isotope pattern), Retention time HPLC: 0.56 min, (X012_S02).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09440930B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-a203165f87654454b3c9f7ab6960ecb7 |
| Source note | uspto-grants-2016_09 |