反应详情

431 mg (0.89 mmol) of 2-chloroethyl 5-{[2-(4-{[(2-chloroethoxy)carbonyl]amino}phenyl)propanoyl]amino}-3cyclopropyl-1H-pyrazole-1-carboxylate were dissolved in 3 ml of N,N-dimethylformamide and 124 mg (0.89 mmol) of potassium carbonate were added and the mixture stirred at room temperature for 19 hours. The reaction mixture was poured into 30 ml of methanol and stirred for 40 minutes, evaporated under vacuum, diluted with 40 ml of methanol and washed with a saturated aqueous ammonium chloride solution. The organic layer was further extracted with dichloromethane, dried over sodium sulfate and evaporated to dryness. The crude was purified by chromatography on a silica gel column to afford 233 mg (77% yield) of the title compound. Analogously, but employing the suitable bisacylated amide derivatives, the following compounds can be prepared:

1. stirringstirred for 40 minutes
2. customevaporated under vacuum
3. additiondiluted with 40 ml of methanol
4. washwashed with a saturated aqueous ammonium chloride solution
5. extractionThe organic layer was further extracted with dichloromethane
6. dry with materialdried over sodium sulfate
7. customevaporated to dryness
8. customThe crude was purified by chromatography on a silica gel column