反应详情

To 20.5 g(0.1 mol) of the compound prepared in Preparation 5-1) in 40 ml of dimethylformamide was added 4.4 g(0.11 mol) of sodium hydride(60%). 18.9 g(0.11 mol) of benzyl bromide was added and the resulting mixture was reacted for 12 hours. After removal of solvent the reaction, solvent was removed and the residue was dissolved in ethylacetate and the organic layer was washed with saturated sodium bicarbonate solution. After removal of solvent, 200 ml of ethanol and 12.5 g(0.25 mol) of hydrazine hydrate was added thereto, and the resulting mixture was refluxed for 3 hours. After the reaction, solvent was removed under reduced pressure. The residue was dissolved in 200 ml of dichloromethane and the organic layer was washed with saturated sodium bicarbonate solution. 200 ml of 1N aqueous hydrochloric acid solution was added and the organic layer was removed. To the aqueous layer was added 200 ml of dichloromethane, and the resulting solution was basified with 6N sodium hydroxide solution. The organic layer was separated and the solvent was removed under reduced pressure to give 8.3 g(Yield 50%) of the title compound.

1. customthe resulting mixture was reacted for 12 hours
2. customAfter removal of solvent
3. customthe reaction, solvent
4. customwas removed
5. dissolutionthe residue was dissolved in ethylacetate
6. washthe organic layer was washed with saturated sodium bicarbonate solution
7. additionwas added
8. temperaturethe resulting mixture was refluxed for 3 hours
9. customAfter the reaction, solvent
10. customwas removed under reduced pressure
11. dissolutionThe residue was dissolved in 200 ml of dichloromethane
12. washthe organic layer was washed with saturated sodium bicarbonate solution
13. addition200 ml of 1N aqueous hydrochloric acid solution was added
14. customthe organic layer was removed
15. additionTo the aqueous layer was added 200 ml of dichloromethane
16. customThe organic layer was separated
17. customthe solvent was removed under reduced pressure