反应详情

2.08 g (3.91 mmol) (2-[2-(3-chloro-pyridin-2-yl)-5-trifluoromethyl-2H-pyrazol-3-yl]-8-hydroxy-6-iodo-benzo[d][1,3]oxazin-4-one (prepared according to WO 04/067528), 0.6 g (4.50 mmol) bicyclopropyl-1-ylamine hydrochloride and 0.63 ml (4.50 mmol) triethylamine in 20 ml THF are heated 20 h at reflux. After cooling down, the precipitate is filtered and the mother liquor is evaporated. The residue is dissolved in 5 ml DMF and poured into 40 ml water. The crystals formed are filtered and purified by flash-chromatography (dichloromethane 40, diethylether 1) to afford 1.85 g title compound. 1H-NMR (CDCl3, 400 MHz. ppm): 0.11 (q, 2H), 0.45 (q, 2H), 0.62 (s, 4H), 1.4 (m, 1H), 2.10 (s, 3H), 6.50 (s, 1H), 7.40 (m, 2H), 7.51 (s, 1H), 7.77 (s, 1H), 7.85 (dd, 1H), 8.49 (m, 1H), 10.45 (s, 1H).

1. temperatureat reflux
2. temperatureAfter cooling down
3. filtrationthe precipitate is filtered
4. customthe mother liquor is evaporated
5. dissolutionThe residue is dissolved in 5 ml DMF
6. additionpoured into 40 ml water
7. customThe crystals formed
8. filtrationare filtered
9. custompurified by flash-chromatography (dichloromethane 40, diethylether 1)