Sodium Carbonate → HCID 9884463, Verbindung

HRID 1084727

Reaktionsgleichung

Reaktionsgleichung von HRID 1084727
[Na].[NH2:2][C:3]1[C:7]([CH3:8])=[CH:6][S:5][C:4]=1C(O)=O.[CH3:12][O:13][C:14]1[CH:15]=[CH:16][CH:17]=[C:18]2[C:23]=1[N:22]=[CH:21][C:20]([C:24]([O:26][CH2:27][CH3:28])=[O:25])=[C:19]2Cl.C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C=CC=CC=1.C(O)C.C(O)(=O)C>[CH3:12][O:13][C:14]1[CH:15]=[CH:16][CH:17]=[C:18]2[C:23]=1[N:22]=[CH:21][C:20]([C:24]([O:26][CH2:27][CH3:28])=[O:25])=[C:19]2[NH:2][C:3]1[C:7]([CH3:8])=[CH:6][S:5][CH:4]=1

Komponenten

8

Edukt 4

HCID 10340Sodium CarbonateHCID 3045573-Quinolinecarboxylic acid, 4-chloro-8-methoxy-, ethyl esterHCID 5360545SodiumHCID 149896783-Amino-4-methylthiophene-2-carboxylic acid

Produkt 1

HCID 9884463HCID 9884463, VerbindungAusbeute 31,4 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 176Acetic AcidLösungsmittelHCID 702EthanolLösungsmittelHCID 1140TolueneLösungsmittel

Versuchsvorschrift

The sodium salt of 3-amino-4-methylthiophene-2-carboxylic acid (7.2 g, 0.04 mol) and ethyl 8-methoxy-4-chloroquinoline-3-carboxylate (5.39 g, 0.02 mol) in toluene (75 ml), ethanol (55 ml) and glacial acetic acid (10 ml) were stirred at room temperature for five days. The solvents were removed by evaporation at reduced pressure to give a dark-green slurry. 10% aqueous sodium carbonate was added and the insoluble solid filtered off, washed well with water and dried. This material was crystallised from ethyl acetate (with charcoaling) to give the title compound as pale yellow crystals (2.15 g), m.p. 162°-164°.

Aufarbeitung

  1. customThe solvents were removed by evaporation at reduced pressure
  2. customto give a dark-green slurry
  3. filtrationthe insoluble solid filtered off
  4. washwashed well with water
  5. customdried
  6. customThis material was crystallised from ethyl acetate (with charcoaling)

Quellen und Nachweise

ORD-Eintrag
ord-87d67d2a1bf3431799652c6e30b4cd43
Quelldatensatz
uspto-grants-1991_04
Patentnummer
US05006535

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