反应详情

1-Methyl-5-(3-chloropropyl)thio-1,2,3,4-tetrazole (1.9 g) and 3-hydroxy-2-mercaptopyridine (1.3 g) are dissolved in acetone (50 ml). To the mixture are added potassium carbonate (1.4 g) and potassium iodide (0.1 g), and the mixture is refluxed for 5 hours. After acetone is distilled off, water is added to the residue, and the mixture is extracted with chloroform. The chloroform solution is washed with saturated aqueous sodium chloride and dried over magnesium sulfate. After chloroform is distilled off, the residue is purified by column chromatography (Kieselgel 60), followed by eluting with chloroform-methanol and recrystallizing from ethyl acetate-n-hexane to give 1-methyl-5-[3-(3-hydroxy-2-pyridyl)thiopropyl]thio-1,2,3,4-tetrazole (1.2 g) as pale yellow granules, m.p. 87.5°-88.5° C.

1. temperaturethe mixture is refluxed for 5 hours
2. distillationAfter acetone is distilled off
3. additionwater is added to the residue
4. extractionthe mixture is extracted with chloroform
5. washThe chloroform solution is washed with saturated aqueous sodium chloride
6. dry with materialdried over magnesium sulfate
7. distillationAfter chloroform is distilled off
8. customthe residue is purified by column chromatography (Kieselgel 60)
9. washby eluting with chloroform-methanol
10. customrecrystallizing from ethyl acetate-n-hexane