[CH3:1][C:2]1[C:7]([CH3:8])=[C:6]([O:9][CH2:10][C:11]([F:14])([F:13])[F:12])[CH:5]=[CH:4][N+:3]=1[O-].[CH3:16][C:17]([O:19]C(C)=O)=[O:18]>C(Cl)Cl.CN(C)C1C=CN=CC=1>[C:17]([O:19][CH2:1][C:2]1[C:7]([CH3:8])=[C:6]([O:9][CH2:10][C:11]([F:14])([F:13])[F:12])[CH:5]=[CH:4][N:3]=1)(=[O:18])[CH3:16]40 ml of 2,3-dimethyl-4-(2,2,2-trifluoroethoxy)pyridine N-oxide (0.078 mole) in methylene chloride were dropwise added to a solution of 28.7 ml acetanhydride and 0.182 g 4-dimethylaminopyridine, then methylene chloride was distilled off and the residue was heated to a temperature of from 90 to 95° C. for 4-5 hours. At the end of the reaction, 3.6 ml of water were added and acetic acid was removed by vacuum distillation to obtain an oil product. The yield was 94-96%, determined by HPLC.
読み込み中…
