HCID 15098931、化合物 → HCID 178482028、化合物
反応式
[CH3:1][N:2]1[C:6]([S:7][CH2:8][CH2:9][CH2:10][C:11](Cl)=[O:12])=[N:5][N:4]=[N:3]1.N1C=CC=CC=1.[SH2:20]>C(Cl)Cl.C(Cl)(Cl)Cl>[CH3:1][N:2]1[C:6]([S:7][CH2:8][CH2:9][CH2:10][C:11]([OH:12])=[S:20])=[N:5][N:4]=[N:3]1参加物
5
実験手順
920 mg of 4-(1-methyltetrazol-5-ylthio)-butyric acid chloride are dissoved in 1.4 ml of absolute methylene chloride and added dropwise at 0° to 5.54 ml of a pyridine/H2S solution in methylene chloride (30 ml of absolute pyridine and 6 g of H2S in 100 ml of methylene chloride). The whole is then stirred for one hour at 0° under a nitrogen atmosphere. The reaction mixture is taken up in chloroform, the aqueous phase is acidified to a pH of 2 using 2N H2SO4 and extraction is carried out twice with chloroform. The combined organic phases are washed twice with 5 ml of 10% NaHCO3 solution. The pH is then adjusted to 3 using 2N H2SO4 and the title compound is extracted several times with chloroform. The title compound is obtained after drying over sodium sulphate and concentrating.