Reacción #1179959

ord-1541abe3578a4d939181ca73c95149d7

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONwas added
  2. 2
    Otroat room temperature
  3. 3
    workup.WAITat 5° C. for 1 hour
  4. 4
    OtroThe crystals precipitated
  5. 5
    Filtraciónwere collected by filtration

Procedimiento

In 20 mL of ethyl acetate was dissolved 10.0 g of 1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-azetidinol, and 20 mL of isopropanol was added thereto, after which 2.60 mL of concentrated nitric acid (61%) was added dropwise thereto at room temperature. To the reaction mixture was added dropwise 60 mL of ethyl acetate, and the resulting mixture was stirred at the same temperature for 1 hour and then at 5° C. for 1 hour. The crystals precipitated were collected by filtration to obtain 11.3 g of 1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-azetidinol nitrate as colorless crystals.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08129535B2uspto-grants-2012_03