HRID1039576

反应详情

EQUATION

反应方程式

HRID 1039576 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

3.0 g (purity: 90%; 16.4 mmol) of 4-hydroxy-3,6-dichloropyridazine, 7.96 g (49.1 mmol) of 3-trifluoromethylphenol, and 2.03 g (purity: 97%; 49.1 mmol) of sodium hydroxide were added to a mixture of 19.1 g of 1,2-dichlorobenzene and 3.0 g of dimethyl sulfoxide and matured at 180° C. for 8 hours. After completion of the reaction, the reaction mixture was cooled to room temperature, and 50 g of pure water was added to the cooled mixture. A 35% aqueous hydrochloric acid solution was added to the resultant mixture so that the pH of the aqueous phase was adjusted to 2.1, and then the deposited solids were taken out by filtration. 25 mL of methyl t-butyl ether was added to the solids to obtain a slurry. The resultant solids were dried under a reduced pressure to obtain 3.32 g of 6-chloro-3-[3-(trifluoromethyl)phenoxy]-4-pyridazinol in the form of pale brown solids (yield: 69.7%).

WORKUP

后处理

  1. customAfter completion of the reaction
  2. filtrationthe deposited solids were taken out by filtration
  3. addition25 mL of methyl t-butyl ether was added to the solids
  4. customto obtain a slurry
  5. customThe resultant solids were dried under a reduced pressure