HRID414613

反应详情

EQUATION

反应方程式

HRID 414613 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a mixture of 2,6-dimethyl-4-bromoanisole (4.14 g) and tetrakis (triphenylphosphine) palladium (0.69 g) in toluene (40 ml) and 2.0 molar aqueous sodium carbonate (20 ml) was added phenylboric acid (2. 7 g) in ethanol (10 ml). The reaction was heated at reflux for 16 hours, at which time a solution of phenylboric acid (1.0 g) in ethanol (3 ml) was added. The reaction was heated at reflux for a further 6 hours and then cooled to 25° C., and 30% hydrogen peroxide (1.0 ml) was added. The mixture was stirred for one hour, then poured into water and extracted with ether. The organic phase was dried and evaporated and the residue was chromatographed on silica gel, eluting with 9:1 hexane either, so as to afford 2,6-dimethyl-4-methoxybiphenyl.

WORKUP

后处理

  1. temperatureThe reaction was heated
  2. additionwas added
  3. temperatureThe reaction was heated
  4. temperatureat reflux for a further 6 hours
  5. extractionextracted with ether
  6. customThe organic phase was dried
  7. customevaporated
  8. customthe residue was chromatographed on silica gel
  9. washeluting with 9:1 hexane either