Ethanol → HCID 12852073, Verbindung

HRID 1248245Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1248245
[NH2:1][C:2]1[CH:27]=[CH:26][CH:25]=[CH:24][C:3]=1[C:4]([NH:6][CH2:7][CH2:8][N:9]1[CH2:14][CH2:13][CH:12]([C:15](=[O:23])[C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=2)[CH2:11][CH2:10]1)=[O:5].C=O.[CH2:30](O)C>[OH-].[Na+].O>[F:22][C:19]1[CH:18]=[CH:17][C:16]([C:15]([CH:12]2[CH2:11][CH2:10][N:9]([CH2:8][CH2:7][N:6]3[C:4](=[O:5])[C:3]4[C:2](=[CH:27][CH:26]=[CH:25][CH:24]=4)[NH:1][CH2:30]3)[CH2:14][CH2:13]2)=[O:23])=[CH:21][CH:20]=1

Komponenten

6

Edukt 3

HCID 702EthanolHCID 712FormaldehydeHCID 30186512-Amino-N-{2-[4-(4-fluorobenzoyl)piperidin-1-yl]ethyl}benzene-1-carboximidic acid

Produkt 1

HCID 12852073HCID 12852073, VerbindungAusbeute 50 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 14798Sodium HydroxideKatalysatorHCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 6.5 parts of 2-amino-N-[2-[4-(4-fluorobenzoyl)-1-piperidinyl]ethyl]benzamide, 0.5 parts of paraformaldehyde, 3 drops of sodium hydroxide solution 50%, 80 parts of ethanol and 10 parts of water is stirred and refluxed overnight. The reaction mixture is allowed to cool to room temperature while stirring. The precipitated product is filtered off, washed with ethanol and crystallized from 200 parts of ethanol, yielding 3.3 parts (50%) of 3-[2-[4-(4-fluorobenzoyl)-1-piperidinyl]ethyl]-2,3-dihydro-4(1H)-quinazolinone; mp. 203.4° C.

Aufarbeitung

  1. temperaturerefluxed overnight
  2. stirringwhile stirring
  3. filtrationThe precipitated product is filtered off
  4. washwashed with ethanol
  5. customcrystallized from 200 parts of ethanol

Quellen und Nachweise

ORD-Eintrag
ord-aab676c4b055434ead20e113ce209b03
Quelldatensatz
uspto-grants-1985_06
Patentnummer
US04522945

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