反应详情

1-Acetoamido-5-mercapto-1H-tetrazole (1.59 g) was dissolved in anhydrous tetrahydrofuran (27 ml), and the mixture was refluxed. 70% Sodium bis(2-methoxyethoxy)aluminum hydride-toluene solution (5 ml) was added dropwise thereto under stirring. After the addition, the mixture was refluxed for 4 hours. The reaction mixture was evaporated under reduced pressure to remove solvent. Ice-water was added to the residue, and the aqueous solution thus obtained was adjusted to pH 3 with 20% sulfuric acid. The mixture was salted out with sodium chloride, and extracted with ethyl acetate. The extracts were washed with a saturated sodium chloride solution, dried and then evaporated to remove solvent. The residue was recrystallized from isopropyl ether-hexane (1:2) to give 0.97 g of 1-ethylamino-5-mercapto-1H-tetrazole as colorless prisms. mp 90°-91° C.

1. temperaturethe mixture was refluxed
2. additionAfter the addition
3. temperaturethe mixture was refluxed for 4 hours
4. customThe reaction mixture was evaporated under reduced pressure
5. customto remove solvent
6. additionIce-water was added to the residue
7. customthe aqueous solution thus obtained
8. extractionextracted with ethyl acetate
9. washThe extracts were washed with a saturated sodium chloride solution
10. customdried
11. customevaporated
12. customto remove solvent
13. customThe residue was recrystallized from isopropyl ether-hexane (1:2)