반응 #62231

반응 방정식

1,2,3-trimethoxybenzene

mono-methylglutarate

→

product

수율 77.0%

5-Oxo-5-(2,3,4-trimethoxy-phenyl)-pentanoic acid methyl ester

수율 77.0%

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
   기타precipitated out
4. 4
   여과The tan colored product was then filtered
5. 5
   세척washed with water
6. 6
   기타dried under vacuum
7. 7
   기타No, purification

실험 절차

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.

출처