反应详情

A suspension of 2-chloro-4-(p-methyl)phenoxy-2-methyl-3-nitrosobutane (V) in dry methanol (120 ml) was heated to reflux and ammonia gas was passed through until all the solid dissolved (2 hours). Filtration and evaporation of solvent gave a brown solid, which was largely freed of impurities by washing with benzene. Recrystallisation from isopropanol (a small inorganic residue remained) gave the ketoxime hydrochloride (IV) (5.27 g, yield 66%) as colourless crystals, m.p. 217°-8° (decomp.).

1. temperaturewas heated
2. temperatureto reflux
3. dissolutiondissolved (2 hours)
4. filtrationFiltration and evaporation of solvent
5. customgave a brown solid, which
6. washby washing with benzene
7. customRecrystallisation from isopropanol (a small inorganic residue