Réaction #91127

ord-fcf6901b84ec4af59fd8f5051bd6f236

Solvants

Conditions de réaction

Température
0°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    workup.STIRRINGthe mixture was stirred
  2. 2
    Températureunder reflux at 80° C. for 16 hours
  3. 3
    ConcentrationThe reactant was concentrated under reduced pressure, and 6 M HCl aqueous solution
  4. 4
    workup.ADDITIONwas added
  5. 5
    FiltrationThe resulting precipitate was filtered
  6. 6
    Autredried

Mode opératoire

After MeOH (20 mL) was added to 2-mercapto-nicotinic acid (1 g, 6 mmol), the mixture was cooled to 0° C., and 6 M NaOH aqueous solution (3.2 mL) was added slowly thereto. The reactant was stirred at 0° C. for 30 minutes. 1-Iodobutane (0.74 mL, 6 mmol) was added to the reactant, and the mixture was stirred under reflux at 80° C. for 16 hours. The reactant was concentrated under reduced pressure, and 6 M HCl aqueous solution was added thereto to adjust the pH of the solution to 7. The resulting precipitate was filtered and dried to obtain the title compound (1.27 g, 93%).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US09447044B2uspto-grants-2016_09