HRID1973049

反应详情

EQUATION

反应方程式

HRID 1973049 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

71 g of 5-(4-nitrophenoxy)-salicylic acid prepared in accordance with Example 1a were hydrogenated at 90° C/100 atms. in 400 ml of ethanol or methanol in the presence of 2.8 g of Raney nickel. The adsorption of hydrogen ceased after 3 hours at the longest. Following the addition of 100 ml of dimethyl acetamide, the catalyst was separated off under heat, water was added at 100° C until a haze began to form, after which the solution was heated for 20 minutes in the presence of 20 g of active carbon and the free aminophenoxy salicylic acid allowed to crystallise out after filtration, being obtained in a yield of 50 g (79% of the theoretical yield), m.p. 223° - 224° C.

WORKUP

后处理

  1. customwere hydrogenated at 90° C
  2. customthe catalyst was separated off
  3. temperatureunder heat
  4. additionwater was added at 100° C until a haze
  5. customto form
  6. temperatureafter which the solution was heated for 20 minutes in the presence of 20 g of active carbon
  7. customto crystallise out
  8. filtrationafter filtration
  9. custombeing obtained in a yield of 50 g (79% of the
  10. customtheoretical yield), m.p. 223° - 224° C.