[CH3:1][N:2]([CH2:12][CH2:13][CH:14]=[O:15])[C:3]([NH:5][C:6]1[S:7][C:8]([CH3:11])=[N:9][N:10]=1)=[O:4].Cl>O>[CH3:11][C:8]1[S:7][C:6]([N:5]2[CH:14]([OH:15])[CH2:13][CH2:12][N:2]([CH3:1])[C:3]2=[O:4])=[N:10][N:9]=1The dimethyl acetal of 3-[1-methyl-3-(5-methyl-1,3,4-thiadiazol-2-yl)ureido]propionaldehyde (15 grams), water (400 ml) and hydrochloric acid (4 ml) are charged into a glass reaction vessel equipped with a mechanical stirrer, thermometer and reflux condenser. The reaction mixture is heated at reflux for a period of about 15 minutes. The reaction mixture is then filtered while hot and the filtrate is cooled to form a precipitate. The precipitate is recovered by filtration, is dried and is recrystallized to yield the desired product tetrahydro-1-(5-methyl-1,3,4-thiadiazol-2-yl)-3-methyl-6-hydroxy-2 (1H)-pyrimidinone.
読み込み中…