o-CRESYL GLYCIDYL ETHER → HCID 53795165, Verbindung

HRID 745507

Reaktionsgleichung

Reaktionsgleichung von HRID 745507
[CH3:1][C:2]1[CH:12]=[CH:11][CH:10]=[CH:9][C:3]=1[O:4][CH2:5][CH:6]1[O:8][CH2:7]1.[CH2:13]([N:20]([CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[CH2:21][C:22]([CH3:25])([NH2:24])[CH3:23])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>C(O)C>[CH3:1][C:2]1[CH:12]=[CH:11][CH:10]=[CH:9][C:3]=1[O:4][CH2:5][CH:6]([OH:8])[CH2:7][NH:24][C:22]([CH3:25])([CH3:23])[CH2:21][N:20]([CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1

Komponenten

4

Edukt 2

HCID 16640o-CRESYL GLYCIDYL ETHERHCID 11777830HCID 11777830, Verbindung

Produkt 1

HCID 53795165HCID 53795165, VerbindungAusbeute 64,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A micture of 4.3 g of 1-(2-methylphenoxy)-2,3-epoxypropane, 7.03 g of N,N-dibenzyl-2-methyl-1,2-propanediamine and 50 ml of ethanol was refluxed for 20 hours, and the solvent was evaporated under reduced pressure. To a benzene solution of the residue was added 1N hydrochloric acid, to deposit an oily material. After removal of the benzene layer, the residue was extracted with chloroform. The organic layer was washed with 5% sodium carbonate and dried over anhydrous sodium sulfate. The solvent was evaporated to give a colorless oily product. The product was chromatographed on a column of silica gel using chloroform as an eluent. 7.3 g of 1-(2-methylphenoxy)-3-(1,1-dimethyl-2-dibenzylaminoethylamino)-2-propanol was obtained from the eluate.

Aufarbeitung

  1. customthe solvent was evaporated under reduced pressure
  2. additionTo a benzene solution of the residue was added 1N hydrochloric acid
  3. customAfter removal of the benzene layer
  4. extractionthe residue was extracted with chloroform
  5. washThe organic layer was washed with 5% sodium carbonate
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvent was evaporated
  8. customto give a colorless oily product
  9. customThe product was chromatographed on a column of silica gel

Quellen und Nachweise

ORD-Eintrag
ord-b1ddc2fef6a8414ba1fdf068d491927b
Quelldatensatz
uspto-grants-1986_07
Patentnummer
US04599333

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