反応 #47981

ord-4212fc3454be402f8e59e3d3b916f038

反応条件

詳細条件
See reaction.notes.procedure_details.

実験手順

Utilizing the general procedure outlined for 6-chloro-4-phenyl-3-(2,2,2-trifluoroethyl)-4-(trifluoromethyl)-3,4-dihydroquinazolin-2(1H)-one, 6-chloro-4-hydroxy-3-(2,2,2-trifluoroethyl)-4-(trifluoromethyl)-3,4-dihydroquinazolin-2(1H)-one (227 mg, 0.65 mmol) was reacted with 3.0M ethyl magnesium bromide (0.9 ml, 2.6 mmol) to afford 6-chloro-4-ethyl-3-(2,2,2-trifluoroethyl)-4-(trifluoromethyl)-3,4-dihydroquinazolin2(1H)-one as a white solid. 1H NMR (d6-DMSO, 400 MHz) δ 7.41 (s, 1H), 7.35 (dd, J=2.4 and 8.6 Hz, 1H), 6.88 (d, J=8.8 Hz, 1H), 4.52 (m, 1H), 4.26 (m, 1H), 2.55 (m, 1H), 2.36 (m, 1H), 0.9 (t, J=6.8 Hz, 3H). Exact Mass (Electrospray, M+H) Calc'd, 361.0537; Found, 361.0532.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07745452B2uspto-grants-2010_06