Acetic Anhydride → 6-Acetamido-4-methyl-beta-carbolin-3-carboxylic acid ethyl ester

HRID 1085449Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1085449
[CH2:1]([O:3][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])[CH3:2].[C:21](OC(=O)C)(=[O:23])[CH3:22]>N1C=CC=CC=1>[CH2:1]([O:3][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]([NH:20][C:21](=[O:23])[CH3:22])=[CH:13][CH:12]=3)=[O:5])[CH3:2]

Komponenten

4

Edukt 2

HCID 7918Acetic AnhydrideHCID 130373386-Amino-4-methyl-beta-carboline-3-carboxylic-acid-ethylester

Produkt 1

HCID 130373396-Acetamido-4-methyl-beta-carbolin-3-carboxylic acid ethyl ester

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

0.6 g of 6-amino-4-methyl-β-carbolin-3-carboxylic acid ethyl ester is dissolved in 6 ml of pyridine and 1.5 ml of acetic anhydride and the whole is stirred for 16 hours at room temperature. The mixture is then stirred into 30 ml of ice water and intensely extracted with ethyl acetate. The extracts are washed until neutral with semisaturated common salt solution, dried using sodium sulphate and filtered. The solvent is distilled off in vacuo. The residue (0.78 g) is recrystallized from acetone-diisopropyl ether. 0.49 g of 6-acetamido-4-methyl-β-carbolin-3-carboxylic acid ethyl ester of melting point 273°-278° C. is obtained.

Aufarbeitung

  1. extractionintensely extracted with ethyl acetate
  2. washThe extracts are washed until neutral with semisaturated common salt solution
  3. customdried
  4. filtrationfiltered
  5. distillationThe solvent is distilled off in vacuo
  6. customThe residue (0.78 g) is recrystallized from acetone-diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-1febac9703384ab9b83da4eba06571fd
Quelldatensatz
uspto-grants-1991_04
Patentnummer
US05010077

Notizen zur Reaktion

Wird geladen…