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

Tetrahydrofuran → N,N-diethyl-N'-{dibenzo[b,e]thiepin-11(6H)-ylidene}-1,3-propanediamine

HRID 1287925
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1287925
[CH2:1]([N:3]([CH2:23][CH3:24])[CH2:4][CH2:5][CH2:6][NH:7][CH:8]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[CH2:12][S:11][C:10]2[CH:19]=[CH:20][CH:21]=[CH:22][C:9]1=2)[CH3:2].O1CCCC1.Cl[O-].[Na+]>O>[CH2:23]([N:3]([CH2:1][CH3:2])[CH2:4][CH2:5][CH2:6][N:7]=[C:8]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[CH2:12][S:11][C:10]2[CH:19]=[CH:20][CH:21]=[CH:22][C:9]1=2)[CH3:24]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 8028TetrahydrofuranHCID 21507033N,N-diethyl-N'-{6,11-dihydro-dibenzo[b,e]thiepin-11-yl}-1,3-propanediamineHCID 23665760Sodium Hypochlorite

Produkt 1

HCID 21507028N,N-diethyl-N'-{dibenzo[b,e]thiepin-11(6H)-ylidene}-1,3-propanediamine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

2.3 G. of N,N-diethyl-N'-{6,11-dihydro-dibenzo[b,e]thiepin-11-yl}-1,3-propanediamine are dissolved in 50 ml. of absolute tetrahydrofuran and treated dropwise, while stirring, with 6 ml. of 14% aqueous sodium hypochlorite solution. The mixture is stirred at 40°-50° C. for 4 hours, cooled and mixed with 100 ml. of water. The organic phase is extracted with ether. The ether extract is dried over sodium sulfate and evaporated under reduced pressure. The residue is purified by chromatography over aluminum oxide using toluene for the elution. There is obtained N,N-diethyl-N'-{dibenzo[b,e]thiepin-11(6H)-ylidene}-1,3-propanediamine which is taken up in acetone and treated with a solution of 0.4 g. of oxalic acid in 10 ml. of absolute acetone. There is thus obtained N,N-diethyl-N'-{dibenzo[b,e]thiepin-11(6H)-ylidene}-1,3-propanediamine oxalate of melting point 130°-133° C.

Aufarbeitung

  1. stirringThe mixture is stirred at 40°-50° C. for 4 hours
  2. temperaturecooled
  3. additionmixed with 100 ml
  4. extractionThe organic phase is extracted with ether
  5. extractionThe ether extract
  6. dry with materialis dried over sodium sulfate
  7. customevaporated under reduced pressure
  8. customThe residue is purified by chromatography over aluminum oxide
  9. washfor the elution

Quellen und Nachweise

ORD-Eintrag
ord-5951698890214e84b24b27598738af2f
Quelldatensatz
uspto-grants-1976_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US03985895

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion