Reacción #62073

ord-806b5bbbada74336bdda5ebd6120fccc

Reactivos

Ninguno

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Extracciónthe mixture extracted with EtOAc (3×100 ml)
  2. 2
    LavadoThe combined organic extracts were then washed with saturated potassium bicarbonate solution (3×100 ml)
  3. 3
    Otrodried
  4. 4
    Filtraciónfiltered
  5. 5
    Concentraciónconcentrated in vacuo

Procedimiento

Thianthren-1-ol (6.5 g, 27.98 mmol) was dissolved in glacial acetic acid (100 ml) and to this solution was added bromine (17.1 μl, 13.99 mmol) in a dropwise fashion over 30 minutes. Water (200 ml) was added to the amber solution and the mixture extracted with EtOAc (3×100 ml). The combined organic extracts were then washed with saturated potassium bicarbonate solution (3×100 ml), dried using MgSO4, filtered and concentrated in vacuo to give the title compound. (7.56 g, 87%). m/z (LC-MS, ESP):, RT=4.92 min, (M++1)=309.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07429660B2uspto-grants-2008_09