反应详情

1-Isopropylidenamino-5-mercapto-1H-tetrazole sodium salt (5.37 g) was dissolved in a mixture of tetrahydrofuran (24 ml) and methanol (24 ml), and sodium borohydride (1.14 g) was added gradually thereto at 5°-6° C. under stirring. The mixture was stirred at the same temperature for one hour, and then at room temperature for one hour. The mixture was evaporated to remove solvent, and the residue was dissolved in icewater. The aqueous solution was adjusted to pH 2.8 with 6N-hydrochloric acid, and the solution was extracted with ethyl acetate (20 ml) three times repeatedly. The extracts were washed with a saturated sodium chloride solution, dried and then evaporated to remove solvent. n-Hexane was added to the residue thus obtained, and crystalline precipitates were collected by filtration. 4.14 g of 1-isopropylamino-5-mercapto-1H-tetrazole were obtained as colorless needles. mp 92°-95° C.

1. additionwas added gradually
2. stirringThe mixture was stirred at the same temperature for one hour
3. customThe mixture was evaporated
4. customto remove solvent
5. dissolutionthe residue was dissolved in icewater
6. extractionthe solution was extracted with ethyl acetate (20 ml) three times repeatedly
7. washThe extracts were washed with a saturated sodium chloride solution
8. customdried
9. customevaporated
10. customto remove solvent
11. additionn-Hexane was added to the residue
12. customthus obtained
13. customcrystalline precipitates
14. filtrationwere collected by filtration