Reacción #159386

ord-ab6d7f67b8be411aa66b359ec94e8dac

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturathe reaction mixture was heated
  2. 2
    Temperaturato reflux for 4 h
  3. 3
    OtroThe solvent was then removed in vacuo
  4. 4
    Lavadowashed with sat. Rochelle salt solution
  5. 5
    SecadoThe organic phase was dried over sodium sulfate
  6. 6
    Otrothe solvent was removed in vacuo
  7. 7
    OtroThe product with the molecular weight of 221.27 (C11H11NO2S) was obtained in this way

Procedimiento

Tin chloride (11.8 g) was added to a solution of 5-cyclopropylethynyl-3-nitrothiophene-2-carboxylic acid methyl ester (6.26 g) in ethanol (250 ml), and the reaction mixture was heated to reflux for 4 h. The solvent was then removed in vacuo, and the residue was taken up again in ethyl acetate and washed with sat. Rochelle salt solution. The organic phase was dried over sodium sulfate and the solvent was removed in vacuo. The product with the molecular weight of 221.27 (C11H11NO2S) was obtained in this way; MS (ESI): 222 (M+H+).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08828991B2uspto-grants-2014_09