反应详情

温度

70 °C

15.6 g of the ethyl ester of 3[(α-methyl-4-chlorobenzylidene amino)oxy] propionic acid obtained by the method described in Example 13 was dissolved in 100 ml of methanol saturated with ammonia at 25° C. This solution was heated at 70° C. in an autoclave for 7 hours. It was then concentrated by evaporation in a vacuum at 40° C. and the semisolid residue was dissolved by means of 200 ml of diethyl ether, 100 ml of benzene, 200 ml of chloroform and 200 ml of methylene chloride. The resulting solution was extracted thrice with dilute sodium hydroxide, then dried over anhydrous sodium sulfate and finally concentrated by evaporation in a vacuum. The residue obtained was recrystallized from a mixture of 50 ml of benzene, 50 ml of chloroform and 25 ml of petroleum ether. Melting point 149° C.-150° C.

1. concentrationIt was then concentrated by evaporation in a vacuum at 40° C.
2. dissolutionthe semisolid residue was dissolved by means of 200 ml of diethyl ether, 100 ml of benzene, 200 ml of chloroform and 200 ml of methylene chloride
3. extractionThe resulting solution was extracted thrice with dilute sodium hydroxide
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationfinally concentrated by evaporation in a vacuum
6. customThe residue obtained
7. customwas recrystallized from a mixture of 50 ml of benzene, 50 ml of chloroform and 25 ml of petroleum ether