反应详情

温度

85 °C

Diethyl bromoterephthalate (30.1 g, 100 mmol), K2CO3 (27.6 g, 200 mmol) and 140 ml of toluene and 140 ml of H2O were placed in a reaction vessel and argon was passed in for 30 minutes. 4-hexyloxyphenylboronic acid (26.7 g, 120 mmol) (cf. B1) and Pd(PPh3)4 (1.16 g, 1 mmol) were subsequently added under protective gas. The yellow-green, turbid mixture was stirred vigorously under a blanket of protective gas at an internal temperature of 85° C. After 7 hours, the reaction was complete. After phase separation, the organic phase was shaken with dilute HCl/H2O (until neutral). The aqueous phase was shaken with toluene and the organic phases were combined. After filtering off any palladium residues, the solution was evaporated. The product was obtained as a yellowish brown oil in sufficient purity (about 85%): 44.7 g (1112%).

1. customwas passed in for 30 minutes
2. customAfter phase separation
3. stirringthe organic phase was shaken with dilute HCl/H2O (until neutral)
4. stirringThe aqueous phase was shaken with toluene
5. filtrationAfter filtering off any palladium residues
6. customthe solution was evaporated
7. customThe product was obtained as a yellowish brown oil in sufficient purity (about 85%)