HRID1029998

反应详情

EQUATION

反应方程式

HRID 1029998 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1.55 g of 10% palladium-on-carbon, 18.8 g (71.9 mmol) of 2-methyl-4-methoxy-5-nitrophenyl mesylate and 120 ml of ethanol were fed into an autoclave (200 ml), and the mixture was then hydrogenated at 50° C. under 50 g/cm2 for 1 hours with stirring. After allowing to cool, palladium-on-carbon was filtered off and the solvent was distilled off under reduced pressure to obtain brown crystals. The crystals thus obtained were recrystallized from ethanol to thereby give 13.4 g (58.2 mmol) of 2-methyl-4-methoxy-5-aminophenyl mesylate in the form of yellow needle-like crystals. The yield was 81%.

WORKUP

后处理

  1. temperatureto cool
  2. filtrationpalladium-on-carbon was filtered off
  3. distillationthe solvent was distilled off under reduced pressure
  4. customto obtain brown crystals
  5. customThe crystals thus obtained
  6. customwere recrystallized from ethanol