Potassium Hydroxide → HCID 178473690, compound

To a solution of potassium hydroxide (13 g) in methanol (200 ml), with cooling it on ice, was added 3-mercapto-1H-1,2,4-triazole (20 g), followed by 3-chloro-2,4-pentanedione (24 ml). Then, mixture was stirred at room temperature overnight. Insoluble materials in the reaction solution were filtered off, and the filtrate was concentrated under reduced pressure. The residue was extracted with ethyl acetate-water. The organic layer was washed with saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then filtered through a small amount of silica gel, which was washed with ethyl acetate. The filtrate was concentrated under reduced pressure. The residue was recrystallized in ethyl acetate-hexane to yield the title compound (33.1 g).

1. filtrationInsoluble materials in the reaction solution were filtered off
2. concentrationthe filtrate was concentrated under reduced pressure
3. extractionThe residue was extracted with ethyl acetate-water
4. washThe organic layer was washed with saturated aqueous sodium chloride solution
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationfiltered through a small amount of silica gel, which
7. washwas washed with ethyl acetate
8. concentrationThe filtrate was concentrated under reduced pressure
9. customThe residue was recrystallized in ethyl acetate-hexane

ORD record

ord-f653f63048d147168ee959c04b1fa124

Source dataset

uspto-grants-2007_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07238720B2