反应详情

1-Methyl-5-mercapto-1,2,3,4-tetrazole (2.4 g) and N,N-diethyl-3-chloropropylamine (3.0 g) are dissolved in acetone (50 ml). To the mixture are added potassium carbonate (2.8 g) and potassium iodide (0.1 g), and the mixture is refluxed for 4 hours. After acetone is distilled off, water is added to the residue and extracted with chloroform. The chloroform solution is washed with saturated aqueous sodium chloride and dried over sodium sulfate. After chloroform is distilled off, the residue is purified by column chromatography (neutral alumina, made by Merck) and eluted with n-hexane to give 1-methyl-5-[3-(N,N-diethylamino)propylthio]-1,2,3,4-tetrazole (1.09 g) as colorless liquid, nD25 =1.5040.

1. temperaturethe mixture is refluxed for 4 hours
2. distillationAfter acetone is distilled off
3. additionwater is added to the residue
4. extractionextracted with chloroform
5. washThe chloroform solution is washed with saturated aqueous sodium chloride
6. dry with materialdried over sodium sulfate
7. distillationAfter chloroform is distilled off
8. customthe residue is purified by column chromatography (neutral alumina, made by Merck)
9. washeluted with n-hexane