HRID279489

反应详情

EQUATION

反应方程式

HRID 279489 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

At first, a 1-liter autoclave equipped with a mechanical stirrer was charged with 200 g (0.84 mol) of 3,5-bis(trifluoromethyl)benzonitrile, 200 ml of methanol, and 6 g of a catalyst (i.e., a carbon powder (50% wet) carrying thereon 5% palladium), followed by introduction of 14 g of liquid ammonia and then introduction of hydrogen to have a pressure of 1 MPa. Then, the reaction mixture was stirred, while the reaction temperature was maintained at 20° C. and while hydrogen was gradually introduced into the autoclave in a manner to maintain the total pressure at 1 MPa. After conducting the reaction for 3 hr, the reaction was stopped, followed by removing the catalyst by filtration. As a result of analyzing the obtained reaction liquid by gas chromatography, 3,5-bis(trifluoromethyl)benzylamine was formed at a yield of 85.1%.

WORKUP

后处理

  1. customAt first, a 1-liter autoclave equipped with a mechanical stirrer
  2. additionwas gradually introduced into the autoclave in a manner
  3. temperatureto maintain the total pressure at 1 MPa
  4. customthe reaction for 3 hr
  5. customby removing the catalyst
  6. filtrationby filtration
  7. customAs a result
  8. customthe obtained reaction liquid by gas chromatography