Hydroxyurea → HCID 178425012, Verbindung

HRID 1484475Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1484475
[OH:1][NH:2][C:3]([NH2:5])=[O:4].[CH3:6][CH:7]([CH3:15])[CH2:8][C:9](=O)[CH2:10][C:11](=O)[CH3:12].[Cl-:16].[NH4+]>Cl.CO>[ClH:16].[CH3:12][C:11]1[N:5]=[C:3]([OH:4])[N+:2]([O-:1])=[C:9]([CH2:8][CH:7]([CH3:15])[CH3:6])[CH:10]=1

Komponenten

6

Edukt 3

HCID 3657HydroxyureaHCID 25517Ammonium ChlorideHCID 763542,4-Heptanedione, 6-methyl-

Produkt 1

HCID 178425012HCID 178425012, VerbindungAusbeute 58 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidLösungsmittelHCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
-11 °C

Versuchsvorschrift

0.20 mol (15.21 g) hydroxy urea were dissolved in 300 ml of M HCl, 300 ml of methanol were added, and 0.20 mol (28.44 g) 6-methyl-2,4-heptanedione were added dropwise while cooling at −12 to −10° C. The solution was allowed to warm slowly to room temperature and stirred over night, then evaporated to dryness. The residue was suspended with 200 ml of acetone, the mixture cooled to below 0° C. in an ice/ethanol bath, the solid filtered off and washed with a little ice-cold acetone. After drying 7.23 g of a product was obtained, which contained 58% of the title compound and 42% of the by-product ammonium chloride.

Aufarbeitung

  1. additionwere added
  2. temperatureto warm slowly to room temperature
  3. customevaporated to dryness
  4. temperaturethe mixture cooled to below 0° C. in an ice/ethanol bath
  5. filtrationthe solid filtered off
  6. washwashed with a little ice-cold acetone
  7. dry with materialAfter drying 7.23 g of a product
  8. customwas obtained

Quellen und Nachweise

ORD-Eintrag
ord-7a2e6175695c4873bd703fc7e5ba2b7d
Quelldatensatz
uspto-grants-2016_08
Patentnummer
US09422247B2

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