Réaction #62231

ord-31bb2fbdf8ae4a799762b97d126b8f44

Solvants

Conditions de réaction

Température
45°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    workup.ADDITIONThe reaction mixture was then poured into a 1000 mL beaker
  2. 2
    workup.STIRRINGstirred well until all the product
  3. 3
    Autreprecipitated out
  4. 4
    FiltrationThe tan colored product was then filtered
  5. 5
    Lavagewashed with water
  6. 6
    Autredried under vacuum
  7. 7
    AutreNo, purification

Mode opératoire

75 g of polyphosphoric acid (Acros) was charged in a 250 mL round bottom flask, followed by addition of 1,2,3-trimethoxybenzene (5.0 g, 29.73 mmol), and mono-methylglutarate (6.516 g, 44.60 mmol). The reaction mixture was stirred mechanically for 2.5 h at 45° C. The reaction mixture was then poured into a 1000 mL beaker containing around 250 mL of ice, and stirred well until all the product precipitated out. The tan colored product was then filtered and washed with water and dried under vacuum. No, purification required at this stage. 6.78 g (77%) of product was obtained, which was pure by NMR.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07429681B2uspto-grants-2008_09