反应详情

Next, 1.22 g (9.10 mmol) of 1-methyl-5-hydroxypyrazole hydrochloride and 1.53 g (15.17 mmol) of triethylamine were added to dichloromethane (30 ml) under ice cooling. To the mixture, the dichloromethane solution (15 ml) of 2-methyl-3,5-dioxo-4-phenyl-2,3,4,5-tetrahydro-1,2,4-triazine-6-carbonyl chloride was slowly added dropwise, and stirred for 30 minutes. The reaction mixture was extracted with chloroform, and the organic layer was washed with water, dried over magnesium sulfate, and concentrated under reduced pressure. The residues obtained were dissolved in acetonitrile (30 ml), added with 0.92 g (9.10 mmol) of triethylamine and 0.05 g (0.61 mmol) of acetone cyanohydrin, and refluxed for 30 minutes under heating. The reaction mixture was concentrated under reduced pressure, and then the residues were dissolved in water and washed with ethyl acetate. The aqueous layer was acidified by using citric acid, extracted with chloroform, dried over magnesium sulfate, and concentrated under reduced pressure. The crystals obtained were washed with methanol to obtain 0.40 g of the target compound (yield 20%).

1. extractionThe reaction mixture was extracted with chloroform
2. washthe organic layer was washed with water
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residues obtained
6. temperaturerefluxed for 30 minutes
7. temperatureunder heating
8. concentrationThe reaction mixture was concentrated under reduced pressure
9. dissolutionthe residues were dissolved in water
10. washwashed with ethyl acetate
11. extractionextracted with chloroform
12. dry with materialdried over magnesium sulfate
13. concentrationconcentrated under reduced pressure
14. customThe crystals obtained
15. washwere washed with methanol