HRID1065077

反应详情

EQUATION

反应方程式

HRID 1065077 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

48.9 g of phenol are dissolved in 500 ml of xylene, and to this solution are added 30.2 g of pulverised potassium hydroxide in an atmosphere of nitrogen. The reaction mixture is stirred and heated to boiling point, while continuously distilling off the water that is formed. After addition of 0.6 g of copper chloride and 100 g of 2,6-diisopropyl-4-bromoaniline, the mixture is stirred for 8 hours at 150°-155° C., then cooled, and filtered with suction. The filtrate is washed with 15% sodium hydroxide solution (150 ml) and with two 150 ml portions of water. The organic phase is separated and dried over sodium sulfate. The solvent is removed by distillation and the product is distilled, affording the compound of the formula ##STR5## with a boiling point of 103°-104° C./0.01 torr and a melting point of 71°-72° C. (after recrystallisation from hexane).

WORKUP

后处理

  1. temperatureheated
  2. distillationwhile continuously distilling off the water that
  3. customis formed
  4. stirringthe mixture is stirred for 8 hours at 150°-155° C.
  5. temperaturecooled
  6. filtrationfiltered with suction
  7. washThe filtrate is washed with 15% sodium hydroxide solution (150 ml) and with two 150 ml portions of water
  8. customThe organic phase is separated
  9. dry with materialdried over sodium sulfate
  10. customThe solvent is removed by distillation
  11. distillationthe product is distilled
  12. customaffording the compound of the formula ##STR5## with a boiling point of 103°-104° C./0.01 torr
  13. customa melting point of 71°-72° C. (after recrystallisation from hexane)