HRID1195479

反应详情

EQUATION

反应方程式

HRID 1195479 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (E)-5-(2,5-dihydroxy-3,4,6-trimethylphenyl)-3-methyl-2-pentenyl acetate (125 mg; 0.43 mmol), (R)-6,6'-dimethyl-2,2'-bis(diphenylphosphino-1,1'-biphenyl (7 mg, 3%) and π-allylpalladium chloride dimer (2.3 mg, 1.5%) in tetrahydrofuran (2 ml) was held at 65° C. for 12 hours. After cooling the solvent was removed and the residue was purified on 3 g of silica gel with hexane/ethyl acetate (99:1). After crystallization from pentane there was obtained 81 mg of (S)-3,4-dihydro-2,5,7,8-tetramethyl-2-vinyl-2H-[1]-benzopyran-6-ol. O.P. 53%.

WORKUP

后处理

  1. temperatureAfter cooling the solvent
  2. customwas removed
  3. customthe residue was purified on 3 g of silica gel with hexane/ethyl acetate (99:1)
  4. customAfter crystallization from pentane