Water → HCID 13193051, Verbindung

HRID 371251Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 371251
[Cl:1][C:2]([Cl:7])([CH2:5][Cl:6])[CH:3]=[O:4].[CH3:8][C:9]1([C:12](=[O:19])[CH2:13][N:14]2[CH:18]=[N:17][CH:16]=[N:15]2)[CH2:11][CH2:10]1.C(=O)([O-])[O-].[K+].[K+].O>O1CCCC1>[Cl:6][CH2:5][C:2]([Cl:7])([Cl:1])[CH:3]([OH:4])[CH:13]([N:14]1[CH:18]=[N:17][CH:16]=[N:15]1)[C:12]([C:9]1([CH3:8])[CH2:10][CH2:11]1)=[O:19]

Komponenten

6

Edukt 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 246232,2,3-TrichloropropionaldehydeHCID 12760574HCID 12760574, Verbindung

Produkt 1

HCID 13193051HCID 13193051, VerbindungAusbeute 30,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

11.3 g of 2,2,3-trichloropropionaldehyde were added dropwise to 9.2 g (0.056 mol) of 1-methyl-1-(1,2,4-triazol-1-yl-acetyl)-cyclopropane in 120 ml of tetrahydrofuran and 13.6 g (0.1 mol) of potassium carbonate, the temperature increasing slightly. The reaction solution was stirred overnight at room temperature and was thereafter introduced into 500 ml of water. The resulting precipitate was filtered off under suction and recrystallized from methanol. 5.5 g (30% of theory) of 1,2,2-trichloro-3-hydroxy-4-(1,2,4-triazol-1-yl)-5-(1-methylcycloprop-1-yl)-pentan-5-one of melting point 182° to 186° C. were obtained.

Aufarbeitung

  1. temperaturethe temperature increasing slightly
  2. filtrationThe resulting precipitate was filtered off under suction
  3. customrecrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-aca94391de4b4fff8248eb8d8c6eaaed
Quelldatensatz
uspto-grants-1985_07
Patentnummer
US04530715

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