反応 #1607708
関連文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08946439B2
反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A 5 mL microwave vial was charged with 1-bromo-3-iodo-5-(trifluoromethoxy)benzene (98 mg, 0.27 mmol), (6-methylpyridin-3-yl)methanamine (50 mg, 0.41 mmol), molybdenum hexacarbonyl (160 mg, 0.61 mmol), palladium acetate (8 mg, 0.036 mmol), 1,8-diazabicyclo[5.4.0]undec-7-ene (120 mg, 0.79 mmol), and 1,4-dioxane (2 mL). The vial was sealed under nitrogen and the reaction was subjected to microwave irradiation at 120° C. for 20 minutes. After cooling, the mixture was purified via flash chromatography to afford the desired product as a white solid. LC-MS: 391.2 [M+1]+; 1H NMR (CDCl3, 400 MHz): 8.43 (d, J=2.1 Hz, 1H), 7.85 (t, J=1.5 Hz, 1H), 7.63-7.61 (m, 2H), 7.52 (s, 1H), 7.16 (d, J=8.0 Hz, 1H), 6.74 (br, 1H), 4.60 (d, J=5.8 Hz, 2H), 2.55 (s, 3H). The vial was sealed under nitrogen irradiation at 120° C. for 20 minutes After cooling the mixture was purified via flash chromatography
ソース ID: ord-29147acebbec4ad09de7fa11e7cdab62