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Sodium Iodide → HCID 12899539, Verbindung

HRID 621561
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 621561
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 84,2 %

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 under stirring conditions. The reactions mixture is concentrated under a reduced pressure to obtain a viscous liquid, then 300 ml of 3% sodium hydrogencarbonate aqueous solution are added. The organic layer is extracted with chloroform and washed with water. After drying the chloroform layer, 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 reactions 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, chloroform
  7. customis removed by distillation
  8. customThe residue thus obtained
  9. washis washed with ether
  10. customrecrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-7c43a7bdc2c4467aab4cc9d06094cd98
Quelldatensatz
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04824840

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