反应详情

Potassium tert-butoxide (1.0 g, 9.06 mmol) was suspended in 1,4-dioxane (20 mL) and treated with methyltriphenylphosphonium bromide (3.2 g, 9.06 mmol). The mixture was allowed to stir at rt for 30 min. A yellow suspension formed then Intermediate AF (1-[4-(4-amino-6-formylpyrrolo[2,1-f][1,2,4]triazin-5-yl)phenyl]-3-[4-(trifluoromethyl)-pyridin-2-yl]urea) (2.0 g, 4.53 mmol) in 1,4-dioxane (10 mL) was slowly added and the reaction was stirred at rt for 4 hr. The reaction was slowly poured into vigorously stirring water. The mixture was allowed to stir for 1 hr. The solid was filtered and rinsed with water and MeOH. A light brown solid was isolated (1.2 g, 60%). 1H-NMR (DMSO-d6) δ 9.90 (s, 1H), 9.77 (s, 1H), 8.53 (d, J=5.2 Hz, 1H), 8.06-8.05 (m, 2H), 7.84 (s, 1H), 7.64 (d, J=8.5 Hz, 2H), 7.36 (d, J=5.4 Hz, 1H), 7.31 (d, J=8.5 Hz, 2H), 6.39 (dd, J1=11.3, J2=17.6 Hz, 1H), 5.63 (dd, J1=1.7, J2=17.5 Hz, 1H), 5.12 (dd, J1=1.5, J2=11.1 Hz, 2H). MS [M+H]+=440.0; LCMS RT=2.88.

1. customA yellow suspension formed
2. stirringthe reaction was stirred at rt for 4 hr
3. stirringto stir for 1 hr
4. filtrationThe solid was filtered
5. washrinsed with water and MeOH
6. customA light brown solid was isolated (1.2 g, 60%)
7. customLCMS RT=2.88