HRID1030321

反应详情

EQUATION

反应方程式

HRID 1030321 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

37.4 g (0.1 mol) of 2-(2'-hydroxy-3',5'-di-t-butylphenyl)-5-chlorobenzotriazole-N-oxide, 100 ml of toluene, 60 ml of 2-butanol, 120 ml of water, 7 g of tributylamine and 5 g of Raney nickel were charged into a 500-ml stainless autoclave equipped with an agitator. After the air in the autoclave had been replaced by hydrogen, the pressure of hydrogen was set to 10 kg/cm2. The temperature of the resultant mixture was increased under agitation to 65° C. at which the mixture was then subjected to reaction for 7 hours until the absorption of hydrogen was stopped. After the reaction had been completed, the autoclave was cooled, and the catalyst was filtered off. After the toluene layer had been separated, most part of toluene was distilled off, and the residual solid was washed with ethanol and then dried to obtain 28.3 g of 2-(2'-hydroxy-3',5'-di-t-butylphenyl)-5-chlorobenzotriazole (yield, 79.2%; melting point, 152° to 154° C.).

WORKUP

后处理

  1. customequipped with an agitator
  2. temperaturethe autoclave was cooled
  3. filtrationthe catalyst was filtered off
  4. customAfter the toluene layer had been separated
  5. distillationmost part of toluene was distilled off
  6. washthe residual solid was washed with ethanol
  7. customdried