HRID1268451

反应详情

EQUATION

反应方程式

HRID 1268451 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a degassed solution of 0.35 g (1.0 mmol) of 2-bromo-5,6 -dihydro-5,5-dimethyl-8-(phenylthio)-naphthalene (Compound A35) and 0.34 g (1.9 mmol) of ethyl 4-vinylbenzoate in 4.0 mL of triethylamine, was added 0.066 g (0.2 mmol) of tri-o-tolylphosphine and then 0.025 g (0.1 mmol) of palladium(II) acetate. The reaction was heated at 90° C. for 2.25 h. The reaction was concentrated in vacua. The residue was purified by flash chromatography (silica, 5% ethyl acetate in hexane), followed by recrystallization using EtOH to afford the title compound as white crystals.

WORKUP

后处理

  1. concentrationThe reaction was concentrated in vacua
  2. customThe residue was purified by flash chromatography (silica, 5% ethyl acetate in hexane)
  3. customfollowed by recrystallization