HRID1530808

反应详情

EQUATION

反应方程式

HRID 1530808 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

At 60 to 70° C. and under atmospheric pressure, 9.2 g of 4-[1-(trifluoromethyl)vinyl]-1-methoxybenzene in 50 ml of glacial acetic acid were hydrogenated in the presence of 0.26 g of Pd/C (10%) until no further uptake was visible. The catalyst was filtered off, the reaction solution was mixed with 22.7 g of aqueous hydrobromic acid (48%) and heated under reflux for 21 h. The reaction solution was concentrated, taken up in ethyl acetate, washed with aqueous sodium hydrogen carbonate, dried and concentrated to give the title product which was reacted further without any purification.

WORKUP

后处理

  1. customAt 60 to 70° C.
  2. filtrationThe catalyst was filtered off
  3. additionthe reaction solution was mixed with 22.7 g of aqueous hydrobromic acid (48%)
  4. temperatureheated
  5. temperatureunder reflux for 21 h
  6. concentrationThe reaction solution was concentrated
  7. washwashed with aqueous sodium hydrogen carbonate
  8. customdried
  9. concentrationconcentrated