反应详情

33.6 g (162 mmol) 4-methoxy-benzoic acid N′-(1-imino-ethyl)-hydrazide are heated to 180° C. for 30 minutes. After cooling the solidified melt is dissolved in 250 mL chloroform and repeatedly extracted with aqueous sodium hydroxide solution. The aqueous phases are combined, washed with chloroform, filtered and adjusted to an acid pH by the addition of glacial acetic acid. The precipitated solid is suction filtered, washed with water and dissolved by heating in chloroform. The solvent is evaporated down and the residue is filtered. The solid is washed with chloroform and diethyl ether.

1. temperatureAfter cooling the solidified melt
2. extractionrepeatedly extracted with aqueous sodium hydroxide solution
3. washwashed with chloroform
4. filtrationfiltered
5. additionadjusted to an acid pH by the addition of glacial acetic acid
6. filtrationfiltered
7. washwashed with water
8. dissolutiondissolved
9. temperatureby heating in chloroform
10. customThe solvent is evaporated down
11. filtrationthe residue is filtered
12. washThe solid is washed with chloroform and diethyl ether