反应详情

To a solution of (S)-5-[(3,5-Bis-trifluoromethyl-benzyl)-(2-methyl-2H-tetrazol-5-yl)-amino]-2,3,4,5,7,8,9,10-octahydro-naphtho[2,3-b]azepine-1-carboxylic acid tert-butyl ester (0.67 mmol) in dichloromethane (18 mL) add trifluoroacetic acid (2 mL). After stirring at room temperature for 1 h, quench with concentrated sodium carbonate (10 mL) and dilute with dichloromethane (20 mL) and water (20 mL). Separate the organic phase and wash the aqueous with dichloromethane (2×10 mL). Dry the combined organics over sodium sulfate, filter, and remove solvent under vacuum. Chromatograph the product over silica gel eluting with ethyl acetate/hexane (5-30%) to afford the title compound as a colorless foam. MS (ES+): 525 (M+H).

1. customquench with concentrated sodium carbonate (10 mL)
2. additiondilute with dichloromethane (20 mL) and water (20 mL)
3. customSeparate the organic phase
4. washwash the aqueous with dichloromethane (2×10 mL)
5. dry with materialDry the combined organics over sodium sulfate
6. filtrationfilter
7. customremove solvent under vacuum