Water → HCID 135816654, Verbindung

HRID 1493174Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1493174
[CH2:1]([N:3]1[CH2:8][CH2:7][N:6]([C:9]2[N:14]=[C:13]3[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][C:12]3=[C:11]([C:21]3[CH:26]=[CH:25][C:24]([O:27]C)=[CH:23][CH:22]=3)[CH:10]=2)[CH2:5][CH2:4]1)[CH3:2].O.[OH-].[Na+].C(=O)([O-])O.[Na+]>Br>[CH2:1]([N:3]1[CH2:8][CH2:7][N:6]([C:9]2[N:14]=[C:13]3[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][C:12]3=[C:11]([C:21]3[CH:26]=[CH:25][C:24]([OH:27])=[CH:23][CH:22]=3)[CH:10]=2)[CH2:5][CH2:4]1)[CH3:2]

Komponenten

6

Edukt 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 15020700HCID 15020700, Verbindung

Produkt 1

HCID 135816654HCID 135816654, VerbindungAusbeute 47,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 260Hydrogen BromideLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

2-(4-Ethyl-1-piperazinyl)-4-(4-methoxyphenyl)-5,6,7,8,9,10-hexahydrocycloocta[b]pyridine (1.3 g) is dissolved in 48% hydrobromic acid (10 ml) and the mixture is stirred at 120° C. for 2 hours. After cooling, water is added thereto and the mixture is neutralized with 1N aqueous sodium hydroxide solution and sodium hydrogen carbonate. The resulting precipitate is collected by filtration, washed with water, and recrystallized from methanol to give the desired product (0.6 g), m.p. 250°-253° C.

Aufarbeitung

  1. temperatureAfter cooling
  2. filtrationThe resulting precipitate is collected by filtration
  3. washwashed with water
  4. customrecrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-fa61085517bf472d93110015086b9c31
Quelldatensatz
uspto-grants-1991_06
Patentnummer
US05021421

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