Réaction #582001

ord-9a063880eded4b8f8b0c8d4ddfc08f59

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températurewas heated at 50° C. for 24 hours
  2. 2
    Températureto cool to room temperature
  3. 3
    Filtrationfiltered
  4. 4
    Lavagethe filter cake washed with acetonitrile
  5. 5
    workup.ADDITIONThe filtrate was diluted to a total volume of 70 mL with acetonitrile

Mode opératoire

(R)-2-methylpyrrolidine (L) tartrate (1.65 g, 7.00 mmol) and 325 mesh powdered K2CO3 (2.03 g, 14.7 mmol) in acetonitrile (60 mL) were heated at 50° C. in a sealed bottle for 24 hours. The mixture was allowed to cool to room temperature and was treated with 3-butynyl 4-methylbenzenesulfonate (1.24 mL, 7.0 mmol). The mixture was stirred for one hour at room temperature and then was heated at 50° C. for 24 hours. The mixture was allowed to cool to room temperature, filtered, and the filter cake washed with acetonitrile. The filtrate was diluted to a total volume of 70 mL with acetonitrile and used as a 0.1M solution in subsequent steps.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07538138B2uspto-grants-2009_05