反应详情

Add sodium carbonate (36 mg, 0.34 mmol) and methyl iodide (0.021 mL, 0.34 mmol) to a solution of (+/−)-isopropyl 5-[(3,5-bistrifluoromethyl-benzyl)-(1H-tetrazol-5-yl)-amino]-8-chloro-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate (98 mg, 0.17 mmol) in dimethylformamide/acetone (1:1) (1 mL). Stir the reaction mixture at room temperature overnight. Then add water and dichloromethane. Separate the layers and wash the organic phase with brine. Dry the organic layer over anhydrous sodium sulfate, filter and remove the solvent under reduced pressure. Purify the residue by flash chromatography, eluting with hexanes/ethyl acetate, to afford the title compound (70 mg, 70%). MS (ES+): 591 (M+H).

1. customSeparate the layers
2. washwash the organic phase with brine
3. dry with materialDry the organic layer over anhydrous sodium sulfate
4. filtrationfilter
5. customremove the solvent under reduced pressure
6. customPurify the residue by flash chromatography
7. washeluting with hexanes/ethyl acetate