Réaction #164523

ord-e1d09784d5e745e89ef2dfc6d17429fa

Conditions de réaction

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

Traitement

  1. 1
    workup.ADDITIONAfter the addition, reaction mixture
  2. 2
    Températuremaintained for 30 hrs
  3. 3
    TempératureThe reaction mixture was cooled to room temperature 28° C.
  4. 4
    Filtrationfiltered
  5. 5
    workup.DISTILLATIONThe solvent was distilled off
  6. 6
    Autreto get the product

Mode opératoire

To 37.63 gm (0.3163 mole) of benzotriazole and 35 gm of potassium carbonate in Dimethylformamide (DMF) (350 ml) was added slowly under stirring 82 gm of 2-chloromethyl-8-(4,6-dimethoxy-pyrimidin-2-yl)-1,4-dioxa-8-azaspiro[4,5]decane (intermediate for compound 7) in DMF (300 ml). After the addition, reaction mixture was heated to 120° C. and maintained for 30 hrs. The reaction mixture was cooled to room temperature 28° C. and filtered. The solvent was distilled off to get the product. It was a thick dark brown liquid. Yield of product was 90%

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08841296B2uspto-grants-2014_09