反应详情

(R)-3-(Aminomethyl)-1-N-Boc-pyrrolidine (994 mg, 4.86 mmol) was added to the stock solution of (Z)-ethyl 3-(dimethylamino)-2-(3-iodobenzoyl)acrylate (Intermediate 24, 0.34M, 13 mL, 4.42 mmol). The reaction mixture was stirred at room temperature overnight. The solvent was removed in vacuo and the residue was dried in a vacuum oven for 1.5 h. The resulting residue was then dissolved in dimethylformamide (8 mL) and potassium carbonate powder (670 mg, 4.86 mmol) was added. The reaction mixture was heated at 60° C. for overnight then cooled to room temperature. Water (50 mL) was added and the suspension was extracted with ethyl acetate (3×50 mL). The organic layers were dried over sodium sulfate, and the solvent was removed in vacuo to give quantitative (R)-ethyl 1-((1-(tert-butoxycarbonyl)pyrrolidin-3-yl)methyl)-6-iodo-4-oxo-1,4-dihydroquinoline-3-carboxylate as a brown sticky solid.

1. customThe solvent was removed in vacuo
2. customthe residue was dried in a vacuum oven for 1.5 h
3. dissolutionThe resulting residue was then dissolved in dimethylformamide (8 mL)
4. temperatureThe reaction mixture was heated at 60° C. for overnight
5. temperaturethen cooled to room temperature
6. extractionthe suspension was extracted with ethyl acetate (3×50 mL)
7. dry with materialThe organic layers were dried over sodium sulfate
8. customthe solvent was removed in vacuo