反应详情

229.405 g (696.6 mmol) of 3,4-bis(2-methylbutyloxy)-1-bromobenzene, 215 g (731 mmol) of 3,4-bis(2-methylbutyloxy)benzeneboronic acid and 202.1 g (1.462 mol) of K2CO3 were suspended in 800 ml of toluene and 800 ml of water and the mixture was saturated with N2 for 1 hour. 1.74 g (1.505 mmol) of Pd(PPh3)4 was subsequently added under protective gas. The turbid, slightly yellowish mixture was stirred vigorously under reflux for about 7 hours under nitrogen. After cooling, the organic phase was stirred with 500 ml of 1% strength NaCN solution. The phases were separated and the organic phase was washed with water, dried over Na2SO4 and evaporated on a rotary evaporator. This gave 339 g (679.7 mmol, 98%) of a light-brown oil which, according to 1H NMR, had a purity of 97% and was used directly in the subsequent reaction.

1. temperatureunder reflux for about 7 hours under nitrogen
2. temperatureAfter cooling
3. customThe phases were separated
4. washthe organic phase was washed with water
5. dry with materialdried over Na2SO4
6. customevaporated on a rotary evaporator
7. customwas used directly in the subsequent reaction