HRID1049495

反应详情

EQUATION

反应方程式

HRID 1049495 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Under an argon atmosphere, to a solution of 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (844 mg) in toluene (50 mL) were added copper (I) chloride (134 mg) and sodium tert-butoxide (130 mg), and the mixture was stirred at room temperature for 5 min. To the obtained yellow suspension were successively added ethyl 3-(6-(((tert-butyldiphenylsilyl)oxy)methyl)pyrimidin-4-yl)-3-cyclopropylacrylate (6.60 g), polymethylhydrosiloxane (8.10 mL) and tert-butyl alcohol (2.56 mL) at room temperature, and the mixture was directly stirred for 7 hr. To the reaction mixture was added methanol, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (6.70 g) as a pale-yellow oil.

WORKUP

后处理

  1. customat room temperature
  2. stirringthe mixture was directly stirred for 7 hr
  3. customthe solvent was evaporated under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane)