Hydrochloric Acid → HCID 178436617, Verbindung

Temperatur

-15 °C

0.12 mol (9.13 g) hydroxy urea were dissolved in 50 ml 2 M HCl, 20 ml of methanol were added and 0.10 mol (11.41 g) 2,4-hexanedione were added dropwise under cooling by approximately −15° C. Further 30 ml of water and 10 ml of methanol were added. The two-phase reaction mixture was allowed to warm up slowly to room temperature and was stirred at room temperature for further 2 h, then evaporated until dryness. The residue was suspended with 50 ml of acetone, the mixture was cooled in an ice/ethanol bath, the solid filtered off and washed with a little ice-cold acetone. After drying 7.88 g crude product were obtained which were recrystallized from 45 ml ethanol wherefrom first an insoluble salt compound was hot filtered off and the product was subsequently recrystallized from the filtrate at −18° C. 3.0 g product were obtained which were again recrystallized from 28 ml ethanol. Finally 2.26 g of the title compound were obtained.

1. customThe two-phase reaction mixture
2. temperatureto warm up slowly to room temperature
3. customevaporated until dryness
4. temperaturethe mixture was cooled in an ice/ethanol bath
5. filtrationthe solid filtered off
6. washwashed with a little ice-cold acetone
7. dry with materialAfter drying 7.88 g crude product
8. customwere obtained which
9. customwere recrystallized from 45 ml ethanol wherefrom first an insoluble salt compound
10. filtrationwas hot filtered off
11. customthe product was subsequently recrystallized from the filtrate at −18° C

ORD-Eintrag

ord-50a2daf9c0e54c48b7f2792b8370b7a7

Quelldatensatz

uspto-grants-2016_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09422247B2