HRID1485050

反应详情

EQUATION

反应方程式

HRID 1485050 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a mixture of 4-iodobenzaldehyde (500 mg), bis(triphenylphosphine)palladium(II) dichloride (75.6 mg), copper(I) iodide (24.6 mg) and dehydrated tetrahydrofuran (10.0 mL), cyclobutylzinc bromide (0.5 mol/L, solution in tetrahydrofuran, 6.46 mL) was added and the mixture was stirred in a sealed tube at 60° C. for 14 hours. After cooling to room temperature, the precipitate was removed by filtration through Celite (registered trademark). The filtrate was concentrated under reduced pressure and thereafter purified by silica gel column chromatography (n-hexane:ethyl acetate=98:2-90:10) to give the titled compound as a colorless oil (225 mg).

WORKUP

后处理

  1. additionwas added
  2. temperatureAfter cooling to room temperature
  3. customthe precipitate was removed by filtration through Celite (registered trademark)
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. custompurified by silica gel column chromatography (n-hexane:ethyl acetate=98:2-90:10)