反応 #62238

反応方程式

1,2,3-trimethoxybenzene

mono-methyl adipate

→

65

収率 93.1%

6-Oxo-6-(2,3,4-trimethoxy-phenyl)-hexanoic acid methyl ester

収率 93.1%

溶媒

反応条件

後処理

1. 1
   その他equipped with a mechanical stirrer
2. 2
   workup.ADDITIONThe reaction mixture was then poured into a 1000 mL beaker
3. 3
   workup.STIRRINGstirred well
4. 4
   その他Tan colored product precipitated out which
5. 5
   ろ過was then filtered
6. 6
   洗浄washed with water
7. 7
   その他dried under vacuum

実験手順

150 g of polyphosphoric acid (Acros) was added to a mixture of 1,2,3-trimethoxybenzene (10.0 g, 59.47 mmol), and mono-methyl adipate (13.04 mL g, 89.20 mmol) in a 250 mL round bottom flask equipped with a mechanical stirrer. The reaction mixture was stirred for 2.5 h at 45° C. The reaction mixture was then poured into a 1000 mL beaker containing around 500 mL of ice, and stirred well. Tan colored product precipitated out which was then filtered and washed with water and dried under vacuum. 17.18 g (93%) of 65 was obtained, which was pure by NMR. Rf: 0.42 (40:60 EtOAc:Hexanes)

出典