Dimethylamine → 6-amino-4-methyl-beta-carbolin-3-carboxylic acid N,N-dimethylamide

HRID 1085452Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1085452
C(O[C:4]([C:6]1[N:7]=[CH:8][C:9]2[NH:10][C:11]3[C:16]([C:17]=2[C:18]=1[CH3:19])=[CH:15][C:14]([NH2:20])=[CH:13][CH:12]=3)=[O:5])C.[CH3:21][NH:22][CH3:23]>C(O)CO>[CH3:21][N:22]([CH3:23])[C:4]([C:6]1[N:7]=[CH:8][C:9]2[NH:10][C:11]3[C:16]([C:17]=2[C:18]=1[CH3:19])=[CH:15][C:14]([NH2:20])=[CH:13][CH:12]=3)=[O:5]

Komponenten

4

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

0.3 g of 6-amino-4-methyl-β-carbolin-3-carboxylic acid ethyl ester is suspended in 5 ml of ethylene glycol and, after the addition of 3 ml of dimethylamine, the whole is heated for 22 hours at 100° C. After cooling, the mixture is poured into 30 ml of ice water, extracted with ethyl acetate, washed with water until neutral, dried using sodium sulphate, filtered and the solvent is distilled off in vacuo. The crude product precipitates as a fine brown powder. 0.2 g of 6-amino-4-methyl-β-carbolin-3-carboxylic acid N,N-dimethylamide of melting point 235°-245° C. (decomposition) is obtained.

Aufarbeitung

  1. temperatureAfter cooling
  2. extractionextracted with ethyl acetate
  3. washwashed with water until neutral,
  4. customdried
  5. filtrationfiltered
  6. distillationthe solvent is distilled off in vacuo
  7. customThe crude product precipitates as a fine brown powder

Quellen und Nachweise

ORD-Eintrag
ord-2b03e3781ff5440695c0099179aa17be
Quelldatensatz
uspto-grants-1991_04
Patentnummer
US05010077

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