Methylhydrazine → HCID 178431791, Verbindung

HRID 1192962Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1192962
C([O:3][C:4](=O)[C:5]([CH3:12])=[C:6](N)[C:7]([F:10])([F:9])[F:8])C.[CH3:14][NH:15][NH2:16]>C(=O)([O-])O.[Na+]>[CH3:14][N:15]1[C:6]([C:7]([F:10])([F:9])[F:8])=[C:5]([CH3:12])[C:4]([OH:3])=[N:16]1

Komponenten

4

Edukt 2

HCID 6061MethylhydrazineHCID 854481573-Amino-4,4,4-trifluoro-2-methyl-but-2-enoic acid ethyl ester

Produkt 1

HCID 178431791HCID 178431791, VerbindungAusbeute 38 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 516892Sodium BicarbonateLösungsmittel

Versuchsvorschrift

3-Amino-4,4,4-trifluoro-2-methyl-but-2-enoic acid ethyl ester (25.5 g, 124 mmol) was cooled to 0° C. and methyl hydrazine (7 ml, 132 mmol) was added dropwise. The mixture was allowed to warm to room temperature and heated to 50° C. for 20 hours. The mixture was allowed to cool to room temperature and was stirred for 16 hours. The mixture was cooled to 0° C. and saturated aqueous sodium hydrogencarbonate solution (50 ml) was added. The solid was removed by filtration and washed with cold water (0° C.) to give the product as a white solid (8.46 g, 38% yield over two steps).

Aufarbeitung

  1. temperatureheated to 50° C. for 20 hours
  2. temperatureto cool to room temperature
  3. temperatureThe mixture was cooled to 0° C.
  4. customThe solid was removed by filtration
  5. washwashed with cold water (0° C.)

Quellen und Nachweise

ORD-Eintrag
ord-39d3b89f973e4447a6db0f5eb7c7cdc0
Quelldatensatz
uspto-grants-2014_03
Patentnummer
US08680290B2

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