HRID628504

反应详情

EQUATION

反应方程式

HRID 628504 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-(4-methoxy-3-methyl-phenyl)-3,4,5-trimethyl-1H-pyrazole (described in Reference Preparation example 33) 7.3 g, 47% hydrobromic acid 50 ml and acetic acid 50 ml was stirred with heating under reflux for thirty hours. The solvent was distilled off and to the resulting residues was added ethyl acetate 400 ml, and the resulting mixture was stirred at room temperature for one hour. The precipitates were filtered and were washed with hexane, and were concentrated under reduced pressure to give 2-methyl-4-(3,4,5-trimethyl-pyrazol-1-yl)-phenol 6.1 g.

WORKUP

后处理

  1. temperaturewith heating
  2. temperatureunder reflux for thirty hours
  3. distillationThe solvent was distilled off and to the resulting residues
  4. additionwas added ethyl acetate 400 ml
  5. stirringthe resulting mixture was stirred at room temperature for one hour
  6. filtrationThe precipitates were filtered
  7. washwere washed with hexane
  8. concentrationwere concentrated under reduced pressure