Реакция #62236

ord-bdb5c2efb4434099bfacdae154ddb13a

Растворители

Условия реакции

Температура
45°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  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
    Другоеwas precipitated out
  4. 4
    ФильтрацияThe tan colored product was then filtered
  5. 5
    Промывкаwashed with water
  6. 6
    Другоеdried under vacuum

Методика

A mixture of 75 g of polyphosphoric acid (Acros), 1,2,3-trimethoxybenzene (5.0 g, 29.73 mmol), and mono-methyl succinate (5.9 g, 44.59 mmol) were mechanically stirred at 45° C. for 2.5 h. The reaction mixture was then poured into a 1000 mL beaker containing round 250 mL of ice, and stirred well until all the product was precipitated out. The tan colored product was then filtered and washed with water and dried under vacuum. 6.1 g (72%) of 55 was obtained, which was pure by NMR.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07429681B2uspto-grants-2008_09