反应详情

3.0 g of propylamine hydrochloride was dissolved in 60 mL of methanol and 2.2 g of 2-amino-oxo-4,5,6,7-tetrahydrobenzothiazole was added. 1.1 mL of propylamine was poured into the mixture to set pH within the range 6.5-7.0. Then 0.7 g of sodium cyanoborohydride was added and the reaction mixture was stirred for 70 hours under nitrogen atmosphere and at ambient temperature. The reaction mixture was diluted with 50 mL of water and 10 mL of conc. hydrochloric acid. Solvents were removed by evaporation, the yellow residue was stirred with ethanol and the solid was removed by filtration. The filtrate was made alkaline with potassium hydroxide solution and the precipitate was again removed by filtration. Filtrate was several times evaporated with ethanol to remove propylamine. The residue was dissolved in hot ethanol and resulting crystals were collected and dried. Reaction product was characterised by NMR spectra.

1. customSolvents were removed by evaporation
2. stirringthe yellow residue was stirred with ethanol
3. customthe solid was removed by filtration
4. customthe precipitate was again removed by filtration
5. customevaporated with ethanol
6. customto remove propylamine
7. dissolutionThe residue was dissolved in hot ethanol
8. customresulting crystals
9. customwere collected
10. customdried
11. customReaction product