反应详情

温度

100 °C

A mixture of 4-fluoro-3-nitrobenzoic acid (300 mg; 1.62 mmol; 1 eq.) and 2,5-dimethylpyrrolidine (Maybridge AC11676DA; 0.70 mL; 5.72 mmol; 3.53 eq.) was stirred at 100° C. for 5 minutes in the MW. The solution was concentrated in vacuo and the residue taken up in water (100 mL). The aqueous phase was washed with diethyl ether (2×20 mL) then acidified to pH 5 with acetic acid. Extraction with diethyl ether (150 mL), drying over magnesium sulfate and concentration in vacuo afforded the title compound (360 mg, 84%) as an orange solid.

1. concentrationThe solution was concentrated in vacuo
2. washThe aqueous phase was washed with diethyl ether (2×20 mL)
3. extractionExtraction with diethyl ether (150 mL)
4. dry with materialdrying over magnesium sulfate and concentration in vacuo