Acefylline → HCID 86734928, Verbindung

HRID 258811

Reaktionsgleichung

Reaktionsgleichung von HRID 258811
[CH:1](=[C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH2:11][CH2:10][NH:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N:18]1([C:29](=[O:30])[C:28]2[N:27]([CH2:31][C:32]([OH:34])=[O:33])[CH:26]=[N:25][C:24]=2[N:22]([CH3:23])[C:20]1=[O:21])[CH3:19]>C(O)CC>[CH:1](=[C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH2:11][CH2:10][NH2+:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1.[N:18]1([C:29](=[O:30])[C:28]2[N:27]([CH2:31][C:32]([O-:34])=[O:33])[CH:26]=[N:25][C:24]=2[N:22]([CH3:23])[C:20]1=[O:21])[CH3:19]

Komponenten

4

Edukt 2

HCID 69550AcefyllineHCID 70634238HCID 70634238, Verbindung

Produkt 1

HCID 86734928HCID 86734928, VerbindungAusbeute 48 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 10311-PropanolLösungsmittel

Versuchsvorschrift

2.21 g. (0.01 mole) of 1-benzal-1,2,3,4-tetrahydroisoquinoline and 2.38 g. (0.01 mole) of theophylline-7-acetic acid are dissolved under boiling in 25 ml. of n-propanol. The undissolved substances is filtered from the hot solution. The clear filtrate is crystallized while the mixture is cooled. The precipitated crystals are filtered out, covered with n-propanol and dried at room temperature. Thus 2.2 g. of 1-benzal-1,2,3,4-tetrahydroisoquinolinium-theophylline-7-acetate yield 48%) are obtained. Mp.: 168°-173° C. After recrystallization from a twofold amount of n-propanol the melting point was 195°-198° C.

Aufarbeitung

  1. filtrationThe undissolved substances is filtered from the hot solution
  2. customThe clear filtrate is crystallized while the mixture
  3. temperatureis cooled
  4. filtrationThe precipitated crystals are filtered out
  5. customdried at room temperature

Quellen und Nachweise

ORD-Eintrag
ord-d139aa97146b4758aebd90d098d8954c
Quelldatensatz
uspto-grants-1977_07
Patentnummer
US04035366

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