Hydrogen Bromide → HCID 136131615, Verbindung

HRID 594019Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 594019
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-38efffff04904a518aa05534f6f68441
Quelldatensatz
uspto-grants-2016_01
Patentnummer
US09242961B2

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