Réaction #155973

ord-6801e119df3b400d8406cd16cd51ab70

Conditions de réaction

Température
120°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    TempératureAfter cooling to room temperature
  2. 2
    Concentrationthe mixture is concentrated
  3. 3
    Autrepartitioned between ethyl acetate (100 mL) and water (100 mL)
  4. 4
    ExtractionThe water layer is extracted with ethyl acetate (100 mL)
  5. 5
    Séchagethe combined organic layers are dried over Na2SO4
  6. 6
    Filtrationfiltered
  7. 7
    Concentrationconcentrated

Mode opératoire

A mixture of 1,4-dioxa-8-azaspiro[4.5]decane (1.76 g), 2-bromo-3-fluoro-5-(trifluoromethyl)-pyridine (2.95 g), N,N-dimethylformamide (50 mL), 1,4-dioxane (75 mL) and triethylamine (5.07 ml) is stirred in a sealed vessel at 120° C. for 1 h. After cooling to room temperature, the mixture is concentrated and partitioned between ethyl acetate (100 mL) and water (100 mL). The water layer is extracted with ethyl acetate (100 mL) and the combined organic layers are dried over Na2SO4, filtered and concentrated to yield the title compound.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08822471B2uspto-grants-2014_09