Ethyl 2-acetylacetoacetate → HCID 57500595, compound

Temperature

120 °C

3-Amino-5-t-butylpyrazole (1.6 g) and ethyl diacetoacetate (1.7 g) were dissolved in acetic acid (5 ml) and stirred for 3 hours at 120° C. The mixture was cooled to room temperature and concentrated under reduced pressure. Ethanol (10 ml) and 5 N sodium hydroxide solution (3 ml) were added to the residue and then stirred for 1 hour at 70° C. The mixture was cooled to room temperature, and water was added to the mixture which was then washed with ethyl acetate. 2 N Hydrochloric acid was added to the aqueous phase until it became acidic, and precipitated crystals were collected by filtration and washed with water and n-hexane. The product was dried under reduced pressure to give the title compound (2.1 g, Y.:78%) as white crystals.

1. temperatureThe mixture was cooled to room temperature
2. concentrationconcentrated under reduced pressure
3. additionEthanol (10 ml) and 5 N sodium hydroxide solution (3 ml) were added to the residue
4. stirringstirred for 1 hour at 70° C
5. temperatureThe mixture was cooled to room temperature
6. additionwater was added to the mixture which
7. washwas then washed with ethyl acetate
8. addition2 N Hydrochloric acid was added to the aqueous phase until it
9. customprecipitated crystals
10. filtrationwere collected by filtration
11. washwashed with water and n-hexane
12. customThe product was dried under reduced pressure

ORD record

ord-ef9378af416c42a7878ba38c5120b5f2

Source dataset

uspto-grants-2008_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07345180B2