[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[N:8]=[C:9]=[S:10].[C:11]([NH:14][NH2:15])(=[O:13])[CH3:12]>O1CCOCC1.CCOCC>[C:11]([NH:14][NH:15][C:9](=[S:10])[NH:8][C:7]1[CH:6]=[CH:5][N:4]=[CH:3][C:2]=1[Br:1])(=[O:13])[CH3:12]3-bromo-4-isothiocyanato-pyridine (1 g, 4.650 mmol) and acetylhydrazine (344.5 mg, 4.650 mmol) were dissolved in dry 1,4-dioxane (10 mL) and stirred at 80° C. for 0.75 hrs. The orange suspension was allowed to cool to RT. The viscous suspension was diluted with ether and the solid was collected by filtration and washed with ether (3×5 mL) to give 2-acetyl-N-(3-bromopyridin-4-yl)hydrazinecarbothioamide as a salmon-pink solid (1.2187 g, 91% Yield). MS (ES−) 288.9.
読み込み中…