Triethylamine → HCID 21190289, Verbindung

HRID 619468

Reaktionsgleichung

Reaktionsgleichung von HRID 619468
[CH3:1][C:2]1[N:3]=[C:4]2[CH:12]=[CH:11][CH:10]=[C:9]3[N:5]2[C:6]=1[C:7](=[O:18])[N:8]3[CH2:13][CH2:14][CH2:15][CH2:16][NH2:17].C(N(CC)CC)C.[F:26][C:27]([F:35])([F:34])[C:28]([F:33])([F:32])[C:29](O)=[O:30]>C(#N)C>[CH3:1][C:2]1[N:3]=[C:4]2[CH:12]=[CH:11][CH:10]=[C:9]3[N:5]2[C:6]=1[C:7](=[O:18])[N:8]3[CH2:13][CH2:14][CH2:15][CH2:16][NH:17][C:29](=[O:30])[C:28]([F:33])([F:32])[C:27]([F:35])([F:34])[F:26]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 62356Pentafluoropropionic acidHCID 211902113-Methyl-1-[4-(amino)butan-1-yl]-1,4,7b-triazacyclopent[cd]inden-2-one

Produkt 1

HCID 21190289HCID 21190289, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a solution of 2.44 g (10.0 mmol) of 3-methyl-1-[4-(amino)butan-1-yl]-1,4,7b-triazacyclopent[cd]inden-2-one and 1.81 ml (13.0 mmol) of triethylamine in 100 ml of acetonitrile was added, while stirring at room temperature, 2.31 g (12.0 mmol) of ethyl ester of pentafluoropropionic acid. The mixture was stirred for 14 hours at the same temperature. The solvent was distilled off. To the residue was added methylene chloride. The mixture was washed with water, which was dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified by column chromatography (eluent:ethyl acetate), and recrystallized from ethyl acetate--hexane to afford 1.53 g (39.1%, a colorless crystals) of the desired compound.

Aufarbeitung

  1. stirringThe mixture was stirred for 14 hours at the same temperature
  2. distillationThe solvent was distilled off
  3. additionTo the residue was added methylene chloride
  4. washThe mixture was washed with water, which
  5. dry with materialwas dried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled off
  7. customthe residue was purified by column chromatography (eluent:ethyl acetate)
  8. customrecrystallized from ethyl acetate
  9. customhexane to afford 1.53 g (39.1%

Quellen und Nachweise

ORD-Eintrag
ord-302c765e62d644f081b29da537605c1f
Quelldatensatz
uspto-grants-1999_09
Patentnummer
US05958942

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