[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10](=O)[CH3:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].CO[CH:15](OC)[NH2:16].O.[NH2:20]N>CN(C)C=O>[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2[NH:20][N:16]=[CH:15][CH:11]=2)=[CH:6][CH:5]=1)([O-:3])=[O:2]A solution of 1-(4-nitrophenyl)ethanone (605.5 mmol) and bis(methyloxy)methanamine (726 mmol) in N,N-dimethylformamide (1000 mL) was stirred for 1 h at 80° C. The reaction was concentrated in vacuo, the residue was dissolved in ethanol (1000 mL) and treated with hydrazine monohydrate (1816 mmol). After the reaction stirred 2 h at 70° C. it was cooled to room temperature and poured into ice-water (2000 mL). Product precipitated out of solution, which was filtered, washed with water (4×500 mL) and dried to provide the title product as a yellow powder (98%). ESMS [M+H]+: 190.2
불러오는 중…
