Reacción #159174

ord-47dd8055b5d549b4a287e9bd0d63a363

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONwas added
  2. 2
    Otrowas quenched by addition of 10% HCl
  3. 3
    ExtracciónThe aqueous phase was extracted with diethyl ether
  4. 4
    LavadoThe organic phase was washed with brine
  5. 5
    Secadothen dried over MgSO4
  6. 6
    Filtraciónfiltered
  7. 7
    Concentraciónconcentrated

Procedimiento

3a,6a-Dihydro-thieno[3,2-b]thiophene-2-carboxylic acid methoxy-methyl-amide (1.955 g, 8.60 mmol) was dissolved in THF. The stirred solution was cooled to 0° C. before methylmagnesium bromide (1.4 M in PhMe, 8.6 mL, 12.04 mmol) was added. The reaction was allowed to gradually warm to RT o/n, then it was quenched by addition of 10% HCl. The aqueous phase was extracted with diethyl ether. The organic phase was washed with brine then dried over MgSO4, filtered and concentrated to afford the title compound (1.98 g, 80%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08822430B2uspto-grants-2014_09