Potassium Carbonate → HCID 22936639, Verbindung

HRID 387723Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 387723
[C:1]([C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[OH:13])[N:9]=[CH:8][CH:7]=[C:6]2[O:14][C:15]1[CH:20]=[CH:19][C:18]([NH:21][C:22]([NH:24][C:25]2[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[CH:27][CH:26]=2)=[O:23])=[CH:17][CH:16]=1)#[N:2].C(=O)([O-])[O-].[K+].[K+].Br[CH2:40][CH2:41][CH2:42][CH2:43][Cl:44]>CN(C)C=O>[C:1]([C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH2:40][CH2:41][CH2:42][CH2:43][Cl:44])[N:9]=[CH:8][CH:7]=[C:6]2[O:14][C:15]1[CH:20]=[CH:19][C:18]([NH:21][C:22]([NH:24][C:25]2[CH:26]=[CH:27][C:28]([O:31][CH3:32])=[CH:29][CH:30]=2)=[O:23])=[CH:17][CH:16]=1)#[N:2]

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 813641-Bromo-4-chlorobutaneHCID 135829399HCID 135829399, Verbindung

Produkt 1

HCID 22936639HCID 22936639, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

N-(4-(6-Cyano-7-hydroxy-4-quinolyl)oxyphenyl)-N′-(4-methoxyphenyl)urea (200 mg), potassium carbonate (65 mg) and 1-bromo-4-chlorobutane (81 μl) were suspended in dimethylformamide (3 ml), and the suspension was heated and stirred for 1 hour and 50 minutes. The reaction solution was poured into saturated saline and extracted with ethyl acetate. After drying the organic layer over magnesium sulfate, it was passed through NH silica (Fuji Silicia Chemical) and washed in ethyl acetate, and the filtrate was concentrated. The obtained solid was washed with ether and dried to obtain 110 mg of the title compound.

Aufarbeitung

  1. temperaturethe suspension was heated
  2. additionThe reaction solution was poured into saturated saline
  3. extractionextracted with ethyl acetate
  4. dry with materialAfter drying the organic layer over magnesium sulfate, it
  5. washwashed in ethyl acetate
  6. concentrationthe filtrate was concentrated
  7. washThe obtained solid was washed with ether
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-ff6f8f1a24f94495bf7cebbcd457bb23
Quelldatensatz
uspto-grants-2013_02
Patentnummer
US08372981B2

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