Reaktion #62236

Reaktionsgleichung

1,2,3-trimethoxybenzene

mono-methyl succinate

→

55

Ausbeute 72.7%

4-Oxo-4-(2,3,4-trimethoxy-phenyl)-butyric acid methyl ester

Ausbeute 72.7%

Lösungsmittel

Reaktionsbedingungen

Aufarbeitung

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
   Sonstigewas precipitated out
4. 4
   FiltrationThe tan colored product was then filtered
5. 5
   Waschenwashed with water
6. 6
   Sonstigedried under vacuum

Vorschrift

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.

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