Hydrogen Bromide → HCID 136131615, Verbindung

HRID 227838Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 227838
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-e5057b0ba54c48b3adb1d48ae359c413
Quelldatensatz
uspto-grants-2009_07
Patentnummer
US07560551B2

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