Potassium Sodium Tartrate → HCID 21891870, Verbindung

HRID 1826857Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1826857
[Cl:1][C:2]1[C:11]([C:12](OCC)=[O:13])=[C:10]([CH2:17][N:18]2[CH2:23][CH2:22][N:21]([CH3:24])[CH2:20][CH2:19]2)[C:9]2[C:4](=[CH:5][C:6]([Cl:27])=[C:7]([O:25][CH3:26])[CH:8]=2)[N:3]=1.[H-].C([Al+]CC(C)C)C(C)C.[C@H](O)(C([O-])=O)[C@@H](O)C([O-])=O.[Na+].[K+]>C(Cl)Cl>[Cl:1][C:2]1[C:11]([CH2:12][OH:13])=[C:10]([CH2:17][N:18]2[CH2:19][CH2:20][N:21]([CH3:24])[CH2:22][CH2:23]2)[C:9]2[C:4](=[CH:5][C:6]([Cl:27])=[C:7]([O:25][CH3:26])[CH:8]=2)[N:3]=1

Komponenten

5

Edukt 3

HCID 9357Potassium Sodium TartrateHCID 21225700DiisobutylaluminumhydrideHCID 21891959HCID 21891959, Verbindung

Produkt 1

HCID 21891870HCID 21891870, VerbindungAusbeute 80,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

ethyl 2,7-dichloro-6-methoxy-4-[(4-methyl-1-piperazinyl)methyl]-3-quinolinecarboxylate (6 g, 14.5 mmol) is dissolved in methylene chloride (120 ml). A molar solution of diisobutylaluminium hydride in methylene chloride (60 ml, 60 mmol) is added slowly. Agitation is carried out for one hour at ambient temperature. The reaction mass is slowly poured into 300 ml of a 20% solution of Rochelle salt. Agitation is carried out for one hour, followed by filtering on celite and decanting; the organic phase is washed with a saturated solution of sodium chloride, dried over magnesium sulphate, filtered and evaporated under reduced pressure. The solid is taken up in isopropyl ether, filtered and dried under vacuum. 4.3 g of sought product (80%) is obtained, in the form of a yellow solid.

Aufarbeitung

  1. waitAgitation is carried out for one hour
  2. filtrationby filtering on celite
  3. customdecanting
  4. washthe organic phase is washed with a saturated solution of sodium chloride
  5. dry with materialdried over magnesium sulphate
  6. filtrationfiltered
  7. customevaporated under reduced pressure
  8. filtrationfiltered
  9. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-a9f3f56d313b4bfe911482606bddad83
Quelldatensatz
uspto-grants-2006_05
Patentnummer
US07053102B2

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