反応 #1880958

反応方程式

veratrol

vinylacetic acid

→

5,6-dimethoxy-3-methylindan-1-one

収率 74.0%

溶媒

反応条件

後処理

1. 1
   workup.STIRRINGAfter 30 minutes (min) of stirring
2. 2
   抽出the product was extracted three times
3. 3
   洗浄The combined organic phases were washed twice
4. 4
   乾燥each time with 100 ml of 2N NaOH, once with 100 ml of water and once with 50 ml of saturated sodium chloride solution, dried over sodium sulfate
5. 5
   その他freed from solvent on a rotary evaporator
6. 6
   その他After recrystallizing the residue (in AcOEt/pentane)

実験手順

A mixture of 19.1 ml (150 mmol) of veratrol and 19.2 ml (225 mmol) of vinylacetic acid in 230 g of 83% polyphosphoric acid was stirred for 15 h at 60° C. and then poured into 500 ml of ice water. After 30 minutes (min) of stirring, the product was extracted three times, each time with 200 ml of ether. The combined organic phases were washed twice, each time with 100 ml of 2N NaOH, once with 100 ml of water and once with 50 ml of saturated sodium chloride solution, dried over sodium sulfate and freed from solvent on a rotary evaporator. After recrystallizing the residue (in AcOEt/pentane), 22.8 g (74%) of 5,6-dimethoxy-3-methylindan-1-one were obtained.

出典