Dimethylformamide → HCID 135715021、化合物

反応式

Cl[CH2:2][C:3]1[N:8]2[CH:9]=[N:10][N:11]=[C:7]2[C:6]2[S:12][CH:13]=[CH:14][C:5]=2[N:4]=1.CN(C)C=[O:18].[OH-].[Na+]>O1CCOCC1>[N:8]1[CH:9]=[N:10][N:11]2[C:7]=1[C:6]1[S:12][CH:13]=[CH:14][C:5]=1[NH:4][C:3](=[O:18])[CH2:2]2

参加物

実験手順

5. 15.2 g of 5-(chloromethyl)thieno[2,3-e][1,2,4]triazolo[4,3-c]pyrimidine are suspended in 650 ml of dioxan and 43 ml of dimethylformamide and cooled to 5° C. 86 ml of 1N sodium hydroxide solution are added thereto within 3 min. and the mixture is stirred at room temperature for 17 h. The reaction mixture is then partitioned between 1.5 l of saturated aqueous sodium chloride solution and 0.7 l of chloroform. The aqueous phase is then made weakly acidic (pH 6) with 12N hydrochloric acid. The mixture is extracted five times with chloroform. The organic extracts are concentrated in a vacuum. The crystalline residue is recrystallized from ethanol. There is obtained 5H-thieno[2,3-f][1,2,4]triazolo[1,5-d][1,4]diazepin-6(7H)-one of m.p. 213°-215° C.