[CH2:1]([O:4][CH2:5][C:6]([C:9]1[CH:14]=[C:13]([Br:15])[CH:12]=[CH:11][C:10]=1[F:16])=[N:7][OH:8])[CH:2]=[CH2:3]>C1(C)C(C)=CC=CC=1>[Br:15][C:13]1[CH:12]=[CH:11][C:10]([F:16])=[C:9]([C:6]23[CH2:5][O:4][CH2:1][CH:2]2[CH2:3][O:8][NH:7]3)[CH:14]=1A solution of 2-(allyloxy)-1-(5-bromo-2-fluorophenyl)ethanone oxime (120 g, 417 mmol) in xylene (2 L) is heated at 140° C. for 6 h. The reaction is cooled and the solvent is removed under reduced pressure to give a solid. The solid is purified by trituration with 9:1 hexanes/MTBE to give the title compound (85 g, 72%). ES/MS m/e (79Br/81Br) 288, 290 (M+1).
読み込み中…