HRID1073073

反应详情

EQUATION

反应方程式

HRID 1073073 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10 g of boric acid are added to a solution of 76 g (0.63 mole) of 3-methylbenzaldehyde and 104.5 g (0.63 mole) of 4-nitroacetophenone in 1 l of xylene, and the mixture is refluxed for 8 hours under a water separator. A further 5 g of boric acid are added, after which the mixture is boiled for a further 8 hours. This process is repeated until the theoretical amount of water has been separated off (2-3 times). The cooled reaction mixture is filtered under suction and the residue is washed with toluene and dried under reduced pressure to give 131 g (77% of theory) of a yellowish brown powder of melting point 130°-132° C.

WORKUP

后处理

  1. temperaturethe mixture is refluxed for 8 hours under a water separator
  2. customhas been separated off (2-3 times)
  3. customThe cooled reaction mixture
  4. filtrationis filtered under suction
  5. washthe residue is washed with toluene
  6. customdried under reduced pressure
  7. customto give 131 g (77% of theory) of a yellowish brown powder of melting point 130°-132° C.