Hydrochloric Acid → HCID 86686555, Verbindung

HRID 1528066

Reaktionsgleichung

Reaktionsgleichung von HRID 1528066
[I:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH:13]=[C:12]([O:14][CH3:15])[C:11](=[O:16])[C:10]([C:17](N(OC)C)=[O:18])=[N:9]2)=[C:4]([O:23][CH3:24])[CH:3]=1.Cl.[CH2:26]1COCC1>>[C:17]([C:10]1[C:11](=[O:16])[C:12]([O:14][CH3:15])=[CH:13][N:8]([C:5]2[CH:6]=[CH:7][C:2]([I:1])=[CH:3][C:4]=2[O:23][CH3:24])[N:9]=1)(=[O:18])[CH3:26]

Komponenten

4

Edukt 3

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 594362051-(4-iodo-2-methoxyphenyl)-N,5-dimethoxy-N-methyl-4-oxo-1,4-dihydropyridazine-3-carboxamide

Produkt 1

HCID 86686555HCID 86686555, Verbindung

Versuchsvorschrift

To a solution of 1-(4-iodo-2-methoxyphenyl)-N,5-dimethoxy-N-methyl-4-oxo-1,4-dihydropyridazine-3-carboxamide (8.90 g) in THF (150 mL) was added dropwise 1M methylmagnesium bromide THF solution (30 mL) at −78° C., and the mixture was stirred for 20 min. To the reaction mixture was added 1M hydrochloric acid, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was washed with ethyl acetate, and recrystallized from methanol/water to give the title compound (5.12 g).

Aufarbeitung

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with water and saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. washThe residue was washed with ethyl acetate
  6. customrecrystallized from methanol/water

Quellen und Nachweise

ORD-Eintrag
ord-f72b8724a7504dfb83551c3d726fef6d
Quelldatensatz
uspto-grants-2015_07
Patentnummer
US09090586B2

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