HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 86615667, compound → HCID 86615666, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 86615667 | HCID 86615667 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | HCID 86615666 | HCID 86615666 | 67% |
Reaction Steps
Heat the mixture of (S)-(4-{5-[(3,5-Bis-trifluoromethyl-benzyl)-(2-methyl-2H-tetrazol-5-yl)-amino]-7,9-dimethyl-8-trifluoromethyl-2,3,4,5-tetrahydro-benzo[b]azepin-1-ylmethyl}-cyclohexyl)-acetic acid methyl ester (0.0950 g, 0.129 mmol) in 5.0 N NaOH (1 mL) and methanol (2 mL) under reflux for 2 h. Evaporate the solvents and re-dissolve in water (10 mL). Adjust to pH=7 by adding 2.0 N HCl. Extract with ethyl acetate (2×10 mL). Combine organic layers, dry over anhydrous sodium sulfate and filter. Remove the solvent under reduced pressure. Chromatograph the residue over silica gel, eluting with ethyl acetate/hexanes (0-100%), to provide the title compound as a white foam (0.0620 g, 67%). MS (ES+): 721 (M+H); 719 (M−H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07786108B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-1e2b4861d248407bb0e51f6782380c5a |
| Source note | uspto-grants-2010_08 |