Reacción #80967

ord-a7eb556908204482bceb93a605ec7ad7

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturawas heated
  2. 2
    Temperaturaat reflux for 3.5 h
  3. 3
    Temperaturato cool
  4. 4
    Filtraciónfiltered
  5. 5
    Otrothe solvent was removed in vacuo

Procedimiento

A mixture of 94.0 g (0.91 mol) of 2-methylpropane-thioamide, 115.7 g (0.91 mol) of 1,3-dichloroacetone, and 109.7 g (0.91 mol) of MgSO4 in 1.6 liters of acetone was heated at reflux for 3.5 h. The resulting mixture was allowed to cool, filtered, and the solvent was removed in vacuo to provide the crude desired compound as a yellow oil. 1H NMR (DMSO-d6) δ1.32 (d, J=7 Hz, 6H), 3.27 (heptet, J=7 Hz, 1H), 4.78 (s, 2H), 7.61 (s, 1H). Mass spectrum: (M+H)+ =176.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05616720uspto-grants-1997_04