HRID358318

反应详情

EQUATION

反应方程式

HRID 358318 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a dry, nitrogen-filled 250 ml single-necked round-bottom flask fitted with a nitrogen inlet and magnetic stirring bar was added 11.8 g (65.5 mmol) of stilbene, 11 g (240 mmol) formic acid, 5 g of 10% Pd on activated carbon (4.7 mmol Pd), 60 ml of absolute ethanol and 100 ml of dry benzene. The reaction vessel was placed in a sonicator so that the liquid level inside the flask matched that of the bath water and in the location that produced the maximum cavitation in the flask. After 1 h the flask was removed and the contents filtered. The solid was washed with chloroform and the combined filtrates concentrated on a rotary evaporator. The residual soild was recrystallized (ethanol-pentane) to give 11.03g (92.5% yield) of bibenzyl mp 51°-51.5° (lit 52.5) (8).

WORKUP

后处理

  1. additionTo a dry, nitrogen-filled 250 ml single-necked round-bottom flask
  2. customfitted with a nitrogen inlet and magnetic stirring bar
  3. customproduced the maximum cavitation in the flask
  4. customAfter 1 h the flask was removed
  5. filtrationthe contents filtered
  6. washThe solid was washed with chloroform
  7. concentrationthe combined filtrates concentrated on a rotary evaporator
  8. customThe residual soild was recrystallized (ethanol-pentane)