HRID628530

反应详情

EQUATION

反应方程式

HRID 628530 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-(4-methoxy-2,5-dimethyl-phenyl)-1-methyl-5-trifluoromethyl-1H-pyrazole (described in Reference Preparation example 85) 3 g, 47% hydrobromic acid 29 ml and acetic acid 29 ml was stirred with heating under reflux for twenty one hours. The solvent was distilled off and to the resulting residues was added ice water 90 ml. The precipitates were filtered and were washed with ice water 90 ml and hexane 100 ml, and then were concentrated under reduced pressure to give 2,5-dimethyl-4-(1-methyl-5-trifluoromethyl-1H-pyrazol-3-yl)-phenol 2.9 g.

WORKUP

后处理

  1. temperaturewith heating
  2. temperatureunder reflux for twenty one hours
  3. distillationThe solvent was distilled off and to the resulting residues
  4. additionwas added ice water 90 ml
  5. filtrationThe precipitates were filtered
  6. washwere washed with ice water 90 ml and hexane 100 ml
  7. concentrationwere concentrated under reduced pressure