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Dimethylamine → 4-Benzyloxy-1-dimethylaminocyclohexanecarbonitrile

HRID 1349382
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1349382
[CH3:1][NH:2][CH3:3].[CH2:4]([O:11][CH:12]1[CH2:17][CH2:16][C:15](=O)[CH2:14][CH2:13]1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.Cl.[CH3:20][NH:21]C.[C-]#N.[K+]>CO>[CH2:4]([O:11][CH:12]1[CH2:17][CH2:16][C:15]([N:2]([CH3:3])[CH3:1])([C:20]#[N:21])[CH2:14][CH2:13]1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 674DimethylamineHCID 9032Potassium CyanideHCID 10473Dimethylamine, hydrochlorideHCID 109873694-(Benzyloxy)cyclohexanone

Produkt 1

HCID 210932404-Benzyloxy-1-dimethylaminocyclohexanecarbonitrile

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887
Methanol
Lösungsmittel

Versuchsvorschrift

A mixture of 130 ml of 7.9 molar aqueous dimethylamine solution, 16 ml of methanol, 20.0 g of 4-benzyloxycyclohexanone, 23.2 g of dimethylamine hydrochloride and 15.3 g of potassium cyanide was stirred for 65 hours at room temperature; extraction was carried out four times using 120 ml of diethyl ether each time, and the combined extracts were concentrated; 100 ml of dichloromethane were added to the residue, the phases were separated, and the organic phases were dried over sodium sulfate, filtered and concentrated. 24.5 g of 4-benzyloxy-1-dimethylaminocyclohexanecarbonitrile were obtained in the form of a yellowish oil which slowly solidified.

Aufarbeitung

  1. extractionextraction
  2. concentrationthe combined extracts were concentrated
  3. addition100 ml of dichloromethane were added to the residue
  4. customthe phases were separated
  5. dry with materialthe organic phases were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-4c61180a1d2c49dba50468e13509358b
Quelldatensatz
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07211694B2

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