反应详情

温度

60 °C

To a solution of (S)-5-{9-[(3,5-bis-trifluoromethyl-benzyl)-(2-methyl-2H-tetrazol-5-yl)-amino]-1,3,6,7,8,9-hexahydro-2-oxa-5-aza-cyclohepta[f]inden-5-yl}-3,3-dimethyl-pentanoic acid methyl ester (0.113 mmol) in methanol (3 mL), add 5 N NaOH (2 mL) and heat to 60° C. After stirring for 6 h, cool the reaction to room temperature, dilute with water (10 mL) and neutralize with 5 M HCl. Extract the organics with ethyl acetate (2×20 mL). Combine the organic portions, dry over sodium sulfate, filter, and remove the solvent under vacuum. Chromatograph the product over silica gel, eluting with ethyl acetate/hexane (20-60%) to afford the title compound as a colorless foam. MS (ES+): 641.3 (M+H).

1. temperaturecool
2. customthe reaction to room temperature
3. extractionExtract the organics with ethyl acetate (2×20 mL)
4. dry with materialCombine the organic portions, dry over sodium sulfate
5. filtrationfilter
6. customremove the solvent under vacuum
7. washChromatograph the product over silica gel, eluting with ethyl acetate/hexane (20-60%)