反应详情

A suspension of 2-chloro-4-(p-methoxy)phenoxy-2-methyl-3-nitrosobutane (V) (4.803 g) in dry methanol (80 ml) was heated to reflux while ammonia gas was passed through until all the solid dissolved (3.5 h). Filtration and removal of solvents gave an off-white solid, which was largely freed of impurities by washing with benzene. Two recrystallisations from isopropanol (a small inorganic residue remained) gave the ketoxime hydrochloride (IV) (2.77 g, yield 53%) as colourless crystals, m.p. 219°-220° (decomp.).

1. temperaturewas heated
2. dissolutiondissolved (3.5 h)
3. filtrationFiltration and removal of solvents
4. customgave an off-white solid, which
5. washby washing with benzene
6. customTwo recrystallisations from isopropanol (a small inorganic residue