Butanedione → 4,5-Dimethyl-2-phenylimidazoline-4,5-diol Hydrochloride

HRID 839130

Reaktionsgleichung

Reaktionsgleichung von HRID 839130
O.[ClH:2].[C:3]([NH2:11])(=[NH:10])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[C:12]([C:15]([CH3:17])=[O:16])([CH3:14])=[O:13].C(O)(C)C.O.C([O-])(=O)C.[Na+]>O>[ClH:2].[CH3:17][C:15]1([OH:16])[C:12]([CH3:14])([OH:13])[NH:11][C:3]([C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=2)=[N:10]1

Komponenten

6

Edukt 4

HCID 650ButanedioneHCID 3776IsopropanolHCID 16219042Benzamidine HCl hydrateHCID 23681166Acetic acid, sodium salt, monohydrate

Produkt 1

HCID 203258984,5-Dimethyl-2-phenylimidazoline-4,5-diol Hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

To 56.4 g (0.323 mole) of benzamidine hydrochloride hydrate in 200 ml of warm water is added with vigorous stirring 40 ml of biacetyl. Within a few minutes a heavy precipitate forms and 150 ml of isopropyl alcohol is added followed by 5.0 g of sodium acetate hydrate dissolved in 15 ml of warm water. Stirring is continued for 4 hours after which time the product, 4,5-dimethyl-2-phenylimidazoline-4,5-diol hydrochloride, is filtered off and washed with isopropyl alcohol. Recrystallization from 95% ethanol gives the pure product, m.p. 162°-165° C (dec.).

Aufarbeitung

  1. filtrationafter which time the product, 4,5-dimethyl-2-phenylimidazoline-4,5-diol hydrochloride, is filtered off
  2. washwashed with isopropyl alcohol
  3. customRecrystallization from 95% ethanol
  4. customgives the pure product, m.p. 162°-165° C (dec.)

Quellen und Nachweise

ORD-Eintrag
ord-8f7774b36d9c43039c71186ef27c33d7
Quelldatensatz
uspto-grants-1978_06
Patentnummer
US04093811

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