Acetic Acid → HCID 178433874, Verbindung

HRID 59619

Reaktionsgleichung

Reaktionsgleichung von HRID 59619
[CH3:1][C:2]1[CH:3]=[C:4]([N:9]2[C:13](=[O:14])[C:12](=[N:15][NH:16][C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([Br:23])[C:18]=3[O:24]C)[C:11]([CH3:26])=[N:10]2)[CH:5]=[CH:6][C:7]=1[CH3:8].C(O)(=O)C.O.C(=O)(O)[O-].[Na+]>Br>[CH3:1][C:2]1[CH:3]=[C:4]([N:9]2[C:13](=[O:14])[C:12](=[N:15][NH:16][C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([Br:23])[C:18]=3[OH:24])[C:11]([CH3:26])=[N:10]2)[CH:5]=[CH:6][C:7]=1[CH3:8]

Komponenten

6

Edukt 4

HCID 176Acetic AcidHCID 962WaterHCID 516892Sodium BicarbonateHCID 1784863784-[(3-bromo-2-methoxyphenyl)hydrazinylidene]-2-(3,4-dimethylphenyl)-5-methylpyrazol-3-one

Produkt 1

HCID 178433874HCID 178433874, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 260Hydrogen BromideLösungsmittel

Versuchsvorschrift

A solution of 1-(3,4-dimethylphenyl)-3-methyl-4-(3-bromo-2-methoxyphenyl)hydrazono-5-pyrazolone(5 g) prepared as in Example 2, in 48% aqueous hydrobromic acid (200 mL) and glacial acetic acid (50 mL) was stirred and heated under reflux for about 80 hours. The reaction mixture was concentrated under vacuum to obtain a thick residue. Water (40 mL) was added and basified to pH 7-8 using saturated solution of sodium bicarbonate (20 mL). The mixture was filtered to give an orange solid, which was washed with water (25 mL) and dried in an oven at about 55° C. to about 60° C. for about 12 hours. Yield: 3.5 g

Aufarbeitung

  1. temperatureheated
  2. temperatureunder reflux for about 80 hours
  3. concentrationThe reaction mixture was concentrated under vacuum
  4. customto obtain a thick residue
  5. filtrationThe mixture was filtered
  6. customto give an orange solid, which
  7. washwas washed with water (25 mL)
  8. customdried in an oven at about 55° C. to about 60° C. for about 12 hours

Quellen und Nachweise

ORD-Eintrag
ord-192beb1209844b92a742a2d9f4b045d0
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09440927B2

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