Trichloroacetyl isocyanate → Methyl 2-({[(trichloroacetyl)amino]carbonyl}amino)thiophene-3-carboxylate
反応式
[CH3:1][O:2][C:3]([C:5]1[CH:9]=[CH:8][S:7][C:6]=1[NH2:10])=[O:4].[Cl:11][C:12]([Cl:19])([Cl:18])[C:13]([N:15]=[C:16]=[O:17])=[O:14]>C1COCC1>[Cl:11][C:12]([Cl:19])([Cl:18])[C:13]([NH:15][C:16]([NH:10][C:6]1[S:7][CH:8]=[CH:9][C:5]=1[C:3]([O:2][CH3:1])=[O:4])=[O:17])=[O:14]参加物
4
実験手順
To a stirred solution of 2-amino-thiophene-3-carboxylic acid methyl ester (1 eq) in anhydrous THF (mL) was added trichloroacetyl isocyanate (1 eq) slowly over a period of 5 min. After the addition was complete, a precipitate formed and the reaction stirred for an additional 1 h. The desired product was obtained by filtration to give methyl 2-({[(trichloroacetyl)amino]carbonyl}amino)thiophene-3-carboxylate (99%) as an off-white solid. The product was used in the next step without any further purification. LC/MS (ES, M+H=345).