HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 86615669, compound → HCID 86615668, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 86615669 | HCID 86615669 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | HCID 86615668 | HCID 86615668 | 88.6% |
Reaction Steps
Heat the mixture of (S)-5-{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-yl}-3,3-dimethyl-pentanoic acid methyl ester (0.120 g, 0.169 mmol) in 5.0 N NaOH (1 mL) and methanol (5 mL) under reflux for 2 h. Evaporate the solvents and re-dissolve in water (10 mL). Adjust to pH=4 by adding 4.0 N HCl. Extract with ethyl acetate (2×10 mL). Combine the 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 white foam (0.104 g, 88%). MS (ES+): 695 (M+H); 693 (M−H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07786108B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-a091cd18ad2d4407862038a1170ed772 |
| Source note | uspto-grants-2010_08 |