反应详情

2,4,6-Trifluorobenzoic acid (9.0 g, 34.1 mmol) and cyclopropylamine (14.65 g, 256 mmol) were stirred in pyridine (300 mL) at 120° C. in a sealed tube for 22 h. The solution was concentrated in vacuo. The residue was taken up in water (30 mL) and the solution was acidified to pH 2-3 with 1N HCl. The resulting precipitate was collected by filtration to yield 5.1 g (47%) of clean desired product as a beige solid. 1H NMR (400 MHz, DMSO-d6): δ 8.05 (s, 1H), 6.65 (d, 1H, J=8.0 Hz), 6.42 (t, 1H, J=10.8 Hz), 2.42-2.48 (m, 1H), 0.76-0.83 (m, 2H), 0.45-0.51 (m, 2H). MS (ES) [m+H] calc'd for C10H9F2NO2, 213; found 213.

1. concentrationThe solution was concentrated in vacuo
2. filtrationThe resulting precipitate was collected by filtration