[C:1]1([N:7]2[CH:11]=[N:10][N:9]=[C:8]2[SH:12])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[CH2:14][C:15]([O-:17])=[O:16].[Na+].[OH-].[Na+].Cl>O.C(O)C>[C:15]([CH2:14][S:12][C:8]1[N:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH:11]=[N:10][N:9]=1)([OH:17])=[O:16]
Into 500 ml of ethanol were suspended 53 g (0.3 mol) of 4-phenyl-3-mercapto-1,2,4-triazole and 44.1 g (0.36 mol) of sodium chloroacetate. Thereto was added an aqueous solution prepared by dissolving 15.5 g (0.36 mol) of sodium hydroxide (purity, 93%) into 60 ml of water. This mixture was kept at 50° C. for 3 hours to-react the reactants. The reaction mixture was allowed to cool to room temperature, neutralized by dropwise adding 31 ml (0.36 mol) of concentrated hydrochloric acid, and then cooled to 10° C. or lower with ice. The resulting precipitate was taken out by filtration. To the precipitate was added 1.5 l of ethanol. This mixture was heated, and the insoluble matter was taken out by filtration. Thereafter recrystallization was conducted with cooling to obtain 32.3 g (0.14 mol) of the desired mercaptoacetic acid derivative. Yield, 45.8%.
Wird geladen…
