Water → HCID 178425601, Verbindung

HRID 1930742Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1930742
[O:1]([CH2:8][C:9]1[NH:10][CH:11]=[C:12]([C:14]2[CH:27]=[CH:26][C:17]([O:18][C:19]3[CH:25]=[CH:24][C:22]([NH2:23])=[CH:21][CH:20]=3)=[CH:16][CH:15]=2)[N:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:28][C:29]1[CH:38]=[CH:37][C:32]([CH2:33][N:34]=[C:35]=[O:36])=[CH:31][CH:30]=1.O.C(OCC)(=O)C>CN(C)C=O.C(OCC)C.C(OCC)(=O)C.C(O)(C)C>[CH3:28][C:29]1[CH:38]=[CH:37][C:32]([CH2:33][NH:34][C:35]([NH:23][C:22]2[CH:21]=[CH:20][C:19]([O:18][C:17]3[CH:26]=[CH:27][C:14]([C:12]4[N:13]=[C:9]([CH2:8][O:1][C:2]5[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=5)[NH:10][CH:11]=4)=[CH:15][CH:16]=3)=[CH:25][CH:24]=2)=[O:36])=[CH:31][CH:30]=1

Komponenten

7

Edukt 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 27333881-(Isocyanatomethyl)-4-methylbenzeneHCID 178507748HCID 178507748, Verbindung

Produkt 1

HCID 178425601HCID 178425601, VerbindungAusbeute 21 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 86632829Ethyl ether ethyl acetate isopropanolLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture containing 4-{4-[2-(phenoxymethyl)-1H-imidazol-4-yl]phenoxy}aniline (0.2 g, 0.56 mmol) and 4-methylbenzylisocyanate (0.17 g, 1.12 mmol) in 3 ml of dimethylformamide is heated at 100° C. for two hours. After returning to ambient temperature 20 ml of water and 30 ml of ethyl acetate are added, followed by extraction then the organic phase is washed with a saturated sodium chloride solution. The organic phase is dried over sodium sulfate, filtered and concentrated to dryness under vacuum. The solid obtained is stirred in 5 ml of a mixture of solvents such as ethyl ether/ethyl acetate/isopropanol 6/3/1. The solid obtained is filtered then dried. A cream-coloured powder is obtained with a yield of 21%.

Aufarbeitung

  1. customAfter returning to ambient temperature
  2. additionare added
  3. extractionfollowed by extraction
  4. washthe organic phase is washed with a saturated sodium chloride solution
  5. dry with materialThe organic phase is dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated to dryness under vacuum
  8. customThe solid obtained
  9. customThe solid obtained
  10. filtrationis filtered
  11. customthen dried
  12. customA cream-coloured powder is obtained with a yield of 21%

Quellen und Nachweise

ORD-Eintrag
ord-5c0fb58a60704955a35090b46c82116f
Quelldatensatz
uspto-grants-2012_05
Patentnummer
US08188133B2

Notizen zur Reaktion

Wird geladen…