تفاعل #554597

معادلة التفاعل

3-bromoanisole

2-biphenylboronic acid

sodium carbonate

→

3-methoxy[1,1′:2′,1″]terphenyl

المردود 90.0%

المذيبات

dimethyl ether

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe resultant was refluxed
2. 2
   درجة الحرارةwhile heating for 8 hours
3. 3
   أخرىan aqueous phase was removed
4. 4
   غسيلAn organic phase was washed with water and saturated brine
5. 5
   تجفيفdried with magnesium sulfate
6. 6
   ترشيحAfter the magnesium sulfate was filtered out
7. 7
   تركيزthe organic phase was concentrated
8. 8
   أخرىThe resulting residue was purified by means of silica gel column chromatography

الإجراء التجريبي

Under an argon atmosphere, 18.7 g of 3-bromoanisole, 23.8 g of 2-biphenylboronic acid and 2.31 g of tetraxis(triphenylphosphine)palladium(0) were placed in a flask. 340 mL of dimethyl ether (DME) and 170 mL of a 2M aqueous sodium carbonate solution were added to this flask, and the resultant was refluxed with stirring while heating for 8 hours. After cooling to room temperature, an aqueous phase was removed. An organic phase was washed with water and saturated brine, and then dried with magnesium sulfate. After the magnesium sulfate was filtered out, the organic phase was concentrated. The resulting residue was purified by means of silica gel column chromatography, whereby 23.4 g (yield: 90%) of intended 3-methoxy[1,1′:2′,1″]terphenyl was obtained.

المصدر