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

Sodium Iodide → HCID 12899539, Verbindung

HRID 569962
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 569962
Cl[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:15]=[CH:14][CH:13]=[C:12]2[C:7]=1[CH2:8][CH2:9][C:10](=[O:16])[NH:11]2.[I-].[Na+].[CH2:19]([N:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.C(=O)([O-])O.[Na+]>C(N(CC)CC)C.CN(C)C=O.CC(C)=O>[CH2:19]([N:26]1[CH2:31][CH2:30][N:29]([CH2:2][CH2:3][CH2:4][O:5][C:6]2[CH:15]=[CH:14][CH:13]=[C:12]3[C:7]=2[CH2:8][CH2:9][C:10](=[O:16])[NH:11]3)[CH2:28][CH2:27]1)[C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 5238Sodium IodideHCID 759941-BenzylpiperazineHCID 516892Sodium BicarbonateHCID 12899139HCID 12899139, Verbindung

Produkt 1

HCID 12899539HCID 12899539, VerbindungAusbeute 84 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 180
Acetone
Lösungsmittel
HCID 6228DimethylformamideLösungsmittel
HCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

24 Grams of 5-(3-chloropropoxy)-3,4-dihydrocarbostyril and 17 g of sodium iodide are mixed with 300 ml of acetone and heated for 3 hours under refluxing conditions. Then, 300 ml of dimethylformamide, 12 g of triethylamine and 18 g of 4-benzylpiperazine are added thereto and the reaction is carried out at 60°-70° C. for 7 hours with stirring conditions. The reaction mixture is concentrated under a reduced pressure to obtain a viscous liquid, then 300 ml of 3% sodium hydrogencarbonate aqueous solution is added. The organic layer is extracted with chloroform and washed with water. After drying the chloroform layer, the chloroform is removed by distillation. The residue thus obtained is washed with ether and recrystallized from methanol to obtain 32 g (yield: 84%) of 5-[3-(4-benzylpiperazinyl)propoxy]-3,4-dihydrocarbostyril in the form of colorless needle-like crystals with a melting point of 157°-159° C.

Aufarbeitung

  1. temperatureheated for 3 hours under refluxing conditions
  2. concentrationThe reaction mixture is concentrated under a reduced pressure
  3. customto obtain a viscous liquid
  4. extractionThe organic layer is extracted with chloroform
  5. washwashed with water
  6. dry with materialAfter drying the chloroform layer
  7. customthe chloroform is removed by distillation
  8. customThe residue thus obtained
  9. washis washed with ether
  10. customrecrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-ab73fd6c939c48f7ac3652024bfcb2d5
Quelldatensatz
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04734416

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion