反応 #62231

反応方程式

1,2,3-trimethoxybenzene

mono-methylglutarate

→

product

収率 77.0%

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

収率 77.0%

溶媒

反応条件

後処理

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
   その他precipitated out
4. 4
   ろ過The tan colored product was then filtered
5. 5
   洗浄washed with water
6. 6
   その他dried under vacuum
7. 7
   その他No, purification

実験手順

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.

出典