StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Ethanol → HCID 67315568, Verbindung

HRID 1012575
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1012575
[C:1]([O:4][CH2:5][CH2:6][N:7]([CH2:19][C:20]1[CH:25]=[CH:24][C:23]([CH2:26][NH2:27])=[CH:22][CH:21]=1)[CH2:8][CH2:9][CH2:10][CH2:11][N:12]([CH2:16][CH2:17][CH3:18])[CH2:13][CH2:14][CH3:15])(=[O:3])[CH3:2].C(O)C.[ClH:31].C(O)C.COCCOC>CC(O)C>[ClH:31].[C:1]([O:4][CH2:5][CH2:6][N:7]([CH2:19][C:20]1[CH:25]=[CH:24][C:23]([CH2:26][NH2:27])=[CH:22][CH:21]=1)[CH2:8][CH2:9][CH2:10][CH2:11][N:12]([CH2:13][CH2:14][CH3:15])[CH2:16][CH2:17][CH3:18])(=[O:3])[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 702EthanolHCID 80711,2-DimethoxyethaneHCID 21887872Ethanol hydrochlorideHCID 67314829HCID 67314829, Verbindung

Produkt 1

HCID 67315568HCID 67315568, VerbindungAusbeute 64 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776
Isopropanol
Lösungsmittel

Versuchsvorschrift

6.95 g (0.0184 mol) of unpurified [(4-aminomethylbenzyl)-(4-dipropylaminobutyl)amino]ethyl acetate (14) synthesized in Example 16 and 50 ml of ethanol were charged in a 300 ml recovery flask. 9.8 g (0.066 mol, 3.6 equivalents) of a 25% hydrochloric acid-ethanol solution was added dropwise to the flask under cooling with ice, the mixture was warmed and stirred at room temperature for two hours. The reaction solution was then concentrated. After the addition of hexane to the residue, the mixture was reconcentrated, thereby obtaining foam-like slightly yellow crystals. After dissolving the crystals in 65 ml of IPA at 70° C., 50 ml of ethylene glycol dimethyl ether was added to the solution at 70° C. After stirring the mixture for one day, the precipitated white crystals were recovered by filtration. The crystals were then washed with ethylene glycol dimethyl ether and dried under reduced pressure, thereby obtaining 5.8 g of [(4-aminomethylbenzyl)-(4-dipropylaminobutyl)amino]ethyl acetate hydrochloride (14a) (yield: 64%). [HPLC: 99.0% (HPLC measurement conditions A)] m.p. 105 to 106° C.

Aufarbeitung

  1. temperatureunder cooling with ice
  2. temperaturethe mixture was warmed
  3. concentrationThe reaction solution was then concentrated
  4. additionAfter the addition of hexane to the residue
  5. customobtaining foam-like slightly yellow crystals
  6. stirringAfter stirring the mixture for one day
  7. filtrationthe precipitated white crystals were recovered by filtration
  8. washThe crystals were then washed with ethylene glycol dimethyl ether
  9. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-6cccd021a24a4f3da9bb00a3f3fa83db
Quelldatensatz
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07977512B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion