반응 #62236

반응 방정식

1,2,3-trimethoxybenzene

mono-methyl succinate

→

55

수율 72.7%

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

수율 72.7%

용매

반응 조건

후처리

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
   기타was precipitated out
4. 4
   여과The tan colored product was then filtered
5. 5
   세척washed with water
6. 6
   기타dried under vacuum

실험 절차

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.

출처