Hydrogen Bromide → HCID 136131615, Verbindung

HRID 2361110Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2361110
Br.[CH2:2]([C:4]1[CH:9]=[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[N:7]=[N:6][C:5]=1[NH:16][C:17]1[CH:22]=[CH:21][C:20]([O:23]C)=[CH:19][CH:18]=1)[CH3:3].C([O-])([O-])=O.[Na+].[Na+]>CC(O)=O>[CH2:2]([C:4]1[CH:9]=[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[N:7]=[N:6][C:5]=1[NH:16][C:17]1[CH:18]=[CH:19][C:20]([OH:23])=[CH:21][CH:22]=1)[CH3:3]

Komponenten

5

Edukt 3

HCID 260Hydrogen BromideHCID 10340Sodium CarbonateHCID 57756259HCID 57756259, Verbindung

Produkt 1

HCID 136131615HCID 136131615, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

A RBF was charged with 13.9 mL of 1:1 AcOH:HBr and 4-ethyl-N-(4-methoxyphenyl)-6-phenylpyridazin-3-amine (1.27 g, 4.16 mmol). The flask was fitted with a reflux condenser and was heated at 140° C. for 4 h. Upon cooling, the reaction mixture was poured into ice water and brought to neutral pH by careful addition of 2M aqueous Na2CO3. The resulting precipitate was filtered, washed with water and dried under vacuum to provide 4-(4-ethyl-6-phenylpyridazin-3-ylamino)phenol as a tan solid. MS m/z=292 [M+H]+. Calc'd for C18H17N3O: 291.35.

Aufarbeitung

  1. customThe flask was fitted with a reflux condenser
  2. temperatureUpon cooling
  3. filtrationThe resulting precipitate was filtered
  4. washwashed with water
  5. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-01564132d6ac496896b448a920f329ab
Quelldatensatz
uspto-grants-2014_04
Patentnummer
US08686155B2

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