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Dimethylamine → HCID 12952964, Verbindung

HRID 2286242
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2286242
[ClH:1].[Cl:2][CH2:3][CH2:4][CH:5]1[CH2:9][N:8]([CH3:10])[C:7](=[NH:11])[N:6]1[CH3:12].[CH3:13][NH:14][CH3:15].C[OH:17]>>[OH2:17].[ClH:2].[ClH:1].[NH:11]=[C:7]1[N:6]([CH3:12])[CH:5]([CH2:4][CH2:3][N:14]([CH3:15])[CH3:13])[CH2:9][N:8]1[CH3:10]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 3

HCID 674DimethylamineHCID 887MethanolHCID 20542259HCID 20542259, Verbindung

Produkt 1

HCID 12952964HCID 12952964, VerbindungAusbeute 26 %

Versuchsvorschrift

To 10.0 g (0.047 mole) of 4-(2-chloroethyl)-2-imino-1,3-dimethylimidazolidine hydrochloride was added 6.8 g (0.15 mole) of dimethylamine in 175 ml of methanol. The mixture was heated in a steel bomb at 100° C. for 15 hours. After concentrating in vacuo, the residue was partitioned between a dilute sodium carbonate solution and chloroform. The organic layer was dried (Na2SO4), filtered, and concentrated in vacuo. The residue was dissolved in ethyl acetate and treated with ethereal HCl. The hydrochloride was recrystallized from ethanol twice, and weighed 3.2 g (26% yield); m.p. 210°-212° C.

Aufarbeitung

  1. concentrationAfter concentrating in vacuo
  2. customthe residue was partitioned between a dilute sodium carbonate solution and chloroform
  3. dry with materialThe organic layer was dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. dissolutionThe residue was dissolved in ethyl acetate
  7. additiontreated with ethereal HCl
  8. customThe hydrochloride was recrystallized from ethanol twice

Quellen und Nachweise

ORD-Eintrag
ord-8bba306ccd2e4e54b5032ca7c589d8ac
Quelldatensatz
uspto-grants-1982_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04327108

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