Acetic Acid → 6-[2-(2,6-dichloro-pyridin-3-yl)-benzoxazol-6-yl]-5-methyl-4,5-dihydro-2H-pyridazin-3-one

HRID 1619978Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1619978
[Cl:1][C:2]1[N:25]=[C:24]([Cl:26])[CH:23]=[CH:22][C:3]=1[C:4]([NH:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[CH:18]([CH3:19])[CH2:17][C:16](=[O:20])[NH:15][N:14]=2)=[CH:9][C:8]=1[OH:21])=O.C1(C)C=CC(S(O)(=O)=O)=CC=1.C(O)(=O)C>O>[Cl:1][C:2]1[C:3]([C:4]2[O:21][C:8]3[CH:9]=[C:10]([C:13]4[CH:18]([CH3:19])[CH2:17][C:16](=[O:20])[NH:15][N:14]=4)[CH:11]=[CH:12][C:7]=3[N:6]=2)=[CH:22][CH:23]=[C:24]([Cl:26])[N:25]=1

Komponenten

5

Edukt 3

HCID 176Acetic Acid2×HCID 6101p-Toluenesulfonic acidHCID 866890692,6-dichloro-N-[2-hydroxy-4-(4-methyl-6-oxo-1,4,5,6-tetrahydro-pyridazin-3-yl)-phenyl]-nicotinamide

Produkt 1

HCID 179935426-[2-(2,6-dichloro-pyridin-3-yl)-benzoxazol-6-yl]-5-methyl-4,5-dihydro-2H-pyridazin-3-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

5.8 g (0.015 mol) 2,6-dichloro-N-[2-hydroxy-4-(4-methyl-6-oxo-1,4,5,6-tetrahydro-pyridazin-3-yl)-phenyl]-nicotinamide, 0.6 g para-toluenesulphonic acid and 60 ml glacial acetic acid are refluxed together for 15 h, then 40 ml glacial acetic acid are eliminated in vacuo and the residue is mixed with water. The precipitate formed is filtered off, washed with ethanol and then recrystallised from dioxane/DMF.

Aufarbeitung

  1. customThe precipitate formed
  2. filtrationis filtered off
  3. washwashed with ethanol
  4. customrecrystallised from dioxane/DMF

Quellen und Nachweise

ORD-Eintrag
ord-4a5c6050643142db82953a27704bf795
Quelldatensatz
uspto-grants-2014_07
Patentnummer
US08772323B2

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