Reaktion #1344591

Reaktionsgleichung

compound

tert-butyl 2-({4-[3-(trifluoromethyl)phenyl]-1,3-thiazol-2-yl}methyl)hydrazinecarboxylate

ethyl 2-[(dimethylamino)methylidene]-4,4,4-trifluoro-3-oxobutanoate

triethylamine

→

title compound

Ausbeute 69.2%

ethyl 5-(trifluoromethyl)-1-({4-[3-(trifluoromethyl)phenyl]-1,3-thiazol-2-yl}methyl)-1H-pyrazole-4-carboxylate

Ausbeute 69.2%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturunder reflux for 16 hr
3. 3
   EinengenThe reaction mixture was concentrated under reduced pressure
4. 4
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
5. 5
   SonstigeThe ethyl acetate layer was separated
6. 6
   Trocknendried over sodium sulfate
7. 7
   Einengenconcentrated under reduced pressure
8. 8
   SonstigeThe residue was purified by column chromatography (carrier: silica gel, eluent: hexane-ethyl acetate)

Vorschrift

A mixture of the compound (0.16 g) obtained in Example 103c, ethyl 2-[(dimethylamino)methylidene]-4,4,4-trifluoro-3-oxobutanoate (0.10 g), triethylamine (0.21 mL) and ethanol (4 mL) was heated under reflux for 16 hr. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in ethyl acetate and saturated brine. The ethyl acetate layer was separated, dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography (carrier: silica gel, eluent: hexane-ethyl acetate) to give the title compound (0.13 g) as a colorless oil.

Quelle