HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → [3-[(3,4-Dichlorophenyl)methyl]-2-(1-methylethyl)-3,4,5,6,7,8-hexahydrocyclohepta[d]imidazol-4-yl]acetic acid ammonia salt
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Triethyl [3-[(3,4-dichlorophenyl)methyl]-2-(1-methylethyl)-3,4,5,6,7,8-hexahydrocyclohepta[d]imidazol-4-yl]methanetricarboxylate | HCID 58460159 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | [3-[(3,4-Dichlorophenyl)methyl]-2-(1-methylethyl)-3,4,5,6,7,8-hexahydrocyclohepta[d]imidazol-4-yl]acetic acid ammonia salt | HCID 67435460 | 132.9% |
Reaction Steps
A mixture of Intermediate 9 (435 mg) and Sodium hydroxide, 2M aq (2.3 mL) in Ethanol (6 mL) was stirred at RT for 5 mins and then at 80° C. for 3 hr. The solvent was concentrated under vacuum, the residue suspended in acetic acid (6.00 mL) and heated at 120° C. for 2 hr. The solvent was removed under vacuum and the residue was purified by reverse phase chromatography using acetonitrile water with an ammonium carbonate modifier. The desired fractions were combined and concentrated under vacuum to give a white solid (210 mg). LC/MS MH+ 395, Rt 2.10 min (5 minute run).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08399444B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-67c14a6356674e8c82aad2628182d589 |
| Source note | uspto-grants-2013_03 |