Reaktion #676851

ord-cefb835a10fc403aba4a957e68633d4f

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGstirred vigorously for 5 min
  2. 2
    SonstigeThe organic phase was immediately separated
  3. 3
    Trocknendried with MgSO4
  4. 4
    Einengenconcentrated

Vorschrift

To a solution of 3,5-dimethylbenzothiophene (Intermediate 12) (5.0 g, 33.8 mmol) in CHCl3 (70 mL), chlorosulfonic acid (5.6 mL, 85 mmol) was added dropwise at −5° C. The reaction mixture was stirred at 0° C. for 3 h before it was poured into a mixture of ice and NaHCO3 and stirred vigorously for 5 min. The organic phase was immediately separated, dried with MgSO4 and concentrated yielding 3.5 g (40%) of the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09233946B2uspto-grants-2016_01