反应详情

To an aqueous solution (150 ml) of 3-cyano-4-methoxyaniline hydrochloride (72 g) were added sodium nitrite (29.7 g), stannous chloride dihydrate (266 g) and con. hydrochloric acid (437 ml) with stirring under ice-cooling. After the completion of the reaction, precipitated crystals were collected by filtration. The crystals were added to water, and the mixture was neutralized with aqueous sodium hydroxide solution, extracted with a mixed solvent of toluene and tert-butanol, washed with water and dried over magnesium sulfate. The solvent was evaporated under reduced pressure to give 44 g of 3-cyano-4-methoxyphenylhydrazine.

1. temperaturecooling
2. customAfter the completion of the reaction
3. customprecipitated crystals
4. filtrationwere collected by filtration
5. additionThe crystals were added to water
6. extractionextracted with a mixed solvent of toluene and tert-butanol
7. washwashed with water
8. dry with materialdried over magnesium sulfate
9. customThe solvent was evaporated under reduced pressure