Choline, hydroxide → HCID 178492086, Verbindung

HRID 1600054

Reaktionsgleichung

Reaktionsgleichung von HRID 1600054
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6](=[O:27])[C:7]3[C:15](=[O:16])[N:14]([C:17]4[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][C:18]=4[CH3:25])[N:13]=[C:12]([OH:26])[C:8]=3[NH:9][C:10]=2[CH:11]=1.[OH-].[OH:29][CH2:30][CH2:31][N+:32]([CH3:35])([CH3:34])[CH3:33]>CO>[OH:29][CH2:30][CH2:31][N+:32]([CH3:35])([CH3:34])[CH3:33].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6](=[O:27])[C:7]3[C:15](=[O:16])[N:14]([C:17]4[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][C:18]=4[CH3:25])[N:13]=[C:12]([OH:26])[C:8]=3[NH:9][C:10]=2[CH:11]=1

Komponenten

4

Edukt 2

HCID 31255Choline, hydroxideHCID 178492085HCID 178492085, Verbindung

Produkt 1

HCID 178492086HCID 178492086, VerbindungAusbeute 81 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a stirred suspension of 7-chloro-4-hydroxy-2-(4-methoxy-2-methylphenyl)-1,2,5,10-tetrahydropyridazino[4,5-b]quinoline-1,10-dione (400 mg, 1.03 mM) in methanol (4 mL) was added choline hydroxide (45% by weight in methanol, 295.6 uL, 1.03 mM). After brief sonication, all solids dissolved and the resulting solution was filtered through a Gelman Glass Acrodisc filter (0.45 um) along with an additional quantity of methanol (8 mL). The filtrate was concentrated to dryness and the residual oil was stirred with isopropanol (15 mL) and ethanol (8 mL) whereupon crystallization occurred. The solids were collected and dried under vacuum at 100° C. overnight to give the title compound (411 mg, 81%) as a yellow solid, mp 229°-230°C.

Aufarbeitung

  1. customAfter brief sonication
  2. dissolutionall solids dissolved
  3. filtrationthe resulting solution was filtered through a Gelman Glass Acrodisc
  4. filtrationfilter (0.45 um) along with an additional quantity of methanol (8 mL)
  5. concentrationThe filtrate was concentrated to dryness
  6. customThe solids were collected
  7. customdried under vacuum at 100° C. overnight

Quellen und Nachweise

ORD-Eintrag
ord-9e8ed5dc30af46549f442167a0e1c8e6
Quelldatensatz
uspto-grants-1998_04
Patentnummer
US05744471

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