Pyridine → HCID 178489100, Verbindung

HRID 1637584Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1637584
[C:1](Cl)(=[O:9])[O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.N[C:12]1[CH:16]=[C:15]([C:17]2[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][CH:18]=2)[NH:14][N:13]=1.[N:25]1C=CC=CC=1>>[CH3:24][O:23][C:20]1[CH:21]=[CH:22][C:17]([C:15]2[NH:14][N:13]=[C:12]([C:1]([O:2][C:3]3[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=3)=[O:9])[C:16]=2[NH2:25])=[CH:18][CH:19]=1

Komponenten

4

Edukt 3

HCID 1049PyridineHCID 15891Phenyl chloroformateHCID 27564693-Amino-5-(4-methoxyphenyl)pyrazole

Produkt 1

HCID 178489100HCID 178489100, Verbindung

Versuchsvorschrift

Phenyl chlorocarbonate (0.87 ml) was added to a solution of 3-amino-5-(4-methoxyphenyl)pyrazole (1.19 g) in pyridine (10 ml), and the mixture was stirred at room temperature for 6 hours. The reaction solution was partitioned between ethyl acetate (50 ml) and water (30 ml), and the organic layer was washed with 1 N hydrochloric acid (50 ml×2), saturated aqueous sodium bicarbonate (50 ml) and saturated brine (50 ml) and then dried over anhydrous magnesium sulfate. Then, the solvent was distilled away. The resulting residue was crystallized from ethyl acetate/hexane to obtain the title compound (0.95 g) as pale yellow crystals (melting point: 286-291° C.).

Aufarbeitung

  1. customThe reaction solution was partitioned between ethyl acetate (50 ml) and water (30 ml)
  2. washthe organic layer was washed with 1 N hydrochloric acid (50 ml×2), saturated aqueous sodium bicarbonate (50 ml) and saturated brine (50 ml)
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationThen, the solvent was distilled away
  5. customThe resulting residue was crystallized from ethyl acetate/hexane

Quellen und Nachweise

ORD-Eintrag
ord-b8e560bfb8a944f396898e061bb4240d
Quelldatensatz
uspto-grants-2000_03
Patentnummer
US06043246

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