Réaction #7539

ord-5c19260c8f004085a305aaa6379d532c

Équation de réaction

OC1CCN(CCOCCc2ccc3ccsc3c2)C1
1-{2-[2-(1-benzothiophen-6-yl)ethoxy]ethyl}-3-pyrrolidinol
O=C(O)C(=O)O
oxalic acid
O=C(O)C(=O)O.OC1CCN(CCOCCc2ccc3ccsc3c2)C1
1-{2-[2-(1-benzothiophen-6-yl)ethoxy]ethyl}-3-pyrrolidinol oxalate
Rendement 66.8%

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    workup.WAITat 5° C. for 1 hour
  2. 2
    AutreThe crystals precipitated
  3. 3
    Filtrationwere collected by filtration
  4. 4
    Lavagewashed with ethyl acetate
  5. 5
    Autredried

Mode opératoire

In 2.0 mL of ethyl acetate was dissolved 0.48 g of 1-{2-[2-(1-benzothiophen-6-yl)ethoxy]ethyl}-3-pyrrolidinol, and to the solution was added a solution of 0.15 g of oxalic acid in 2.8 mL of ethyl acetate. The resulting mixture was stirred at room temperature for 1 hour and then at 5° C. for 1 hour. The crystals precipitated were collected by filtration, washed with ethyl acetate and then dried to obtain 0.42 g of 1-{2-[2-(1-benzothiophen-6-yl)ethoxy]ethyl}-3-pyrrolidinol oxalate as colorless crystals.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07087594B2uspto-grants-2006_08