N-Methyl-D-glucamine → HCID 178484187, Verbindung

HRID 323637

Reaktionsgleichung

Reaktionsgleichung von HRID 323637
[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.[CH3:28][NH:29][CH2:30][C@@H:31]([C@H:33]([C@@H:35]([C@@H:37]([CH2:39][OH:40])[OH:38])[OH:36])[OH:34])[OH:32]>CO>[CH3:28][NH:29][CH2:30][C@@H:31]([C@H:33]([C@@H:35]([C@@H:37]([CH2:39][OH:40])[OH:38])[OH:36])[OH:34])[OH:32].[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 8567N-Methyl-D-glucamineHCID 178492085HCID 178492085, Verbindung

Produkt 1

HCID 178484187HCID 178484187, VerbindungAusbeute 29,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

7-Chloro-4-hydroxy-2-(4-methoxy-2-methylphenyl)-1,2,5,10-tetrahydropyridazino[4,5-b]quinoline-1,10-dione (0.45 g, 1.17 mM) was stirred in methanol (20 mL) and N-Methyl-D-Glucamine (0.23 g, 1.17 mM) was added to give a clear yellow solution. This solution was concentrated and the residue was dissolved in water (20 mL) to give a yellow solution. This solution was filtered through a Gellman 0.45 μm Acrodisc and concentrated to give a yellow residue. The residue was triturated with 2-propanol (20 mL) to give a yellow suspension. The solids were collected and washed with 2-propanol to give the title compound (0.20 g, 29%) as a yellow powder, mp 177° C. (decomp.).

Aufarbeitung

  1. customto give a clear yellow solution
  2. concentrationThis solution was concentrated
  3. dissolutionthe residue was dissolved in water (20 mL)
  4. customto give a yellow solution
  5. filtrationThis solution was filtered through a Gellman 0.45 μm Acrodisc
  6. concentrationconcentrated
  7. customto give a yellow residue
  8. customThe residue was triturated with 2-propanol (20 mL)
  9. customto give a yellow suspension
  10. customThe solids were collected
  11. washwashed with 2-propanol

Quellen und Nachweise

ORD-Eintrag
ord-31fd4c9a71da4f0caf55d49f50d289e1
Quelldatensatz
uspto-grants-2001_04
Patentnummer
US06214826B1

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