t-Butyl 4-Fluoroacetoacetate → HCID 178516166, Verbindung

HRID 2050763

Reaktionsgleichung

Reaktionsgleichung von HRID 2050763
[F:1][CH2:2][C:3](=O)[CH2:4][C:5]([O:7]C(C)(C)C)=O.[NH2:13][C:14]1[N:18]=[C:17]([S:19][CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[NH:16][N:15]=1>C(O)(=O)C>[CH2:20]([S:19][C:17]1[N:18]=[C:14]2[N:13]=[C:3]([CH2:2][F:1])[CH:4]=[C:5]([OH:7])[N:15]2[N:16]=1)[C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1

Komponenten

4

Edukt 2

HCID 15029427t-Butyl 4-FluoroacetoacetateHCID 178509291HCID 178509291, Verbindung

Produkt 1

HCID 178516166HCID 178516166, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A solution containing 20.0 g (114 mmol) of t-butyl 4-fluoroacetoacetate, 23.4 g (114 mmol) of 3-amino-5-benzylthio-1,2,4-triazole in 250 ml of glacial acetic acid was heated at reflux with stirring for 5.5 hr and then allowed to cool and stand overnight. The crystals that formed were ground to reduce their size and then recovered by filtration and dried in a vacuum oven to obtain 18.3 g (55 percent of theory) of the title product as a white powder melting with decomposition at 214°-218° C.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux
  3. temperatureto cool
  4. waitstand overnight
  5. customThe crystals that formed
  6. filtrationrecovered by filtration
  7. customdried in a vacuum oven

Quellen und Nachweise

ORD-Eintrag
ord-8204a58ff2c74df997e4f4fe7f0260a4
Quelldatensatz
uspto-grants-1991_05
Patentnummer
US05015286

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