تفاعل #1880958

معادلة التفاعل

veratrol

vinylacetic acid

→

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

المردود 74.0%

المذيبات

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGAfter 30 minutes (min) of stirring
2. 2
   استخلاصthe product was extracted three times
3. 3
   غسيلThe combined organic phases were washed twice
4. 4
   تجفيفeach 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
   أخرىfreed from solvent on a rotary evaporator
6. 6
   أخرىAfter recrystallizing the residue (in AcOEt/pentane)

الإجراء التجريبي

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.

المصدر