Ammonia → 3-Amino-1-phenoxy-3-methylbutan-2-one oxime hydrochloride
反応式
[Cl:1][C:2]([CH3:15])([CH:4]([N:13]=[O:14])[CH2:5][O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[CH3:3].[NH3:16]>CO>[ClH:1].[NH2:16][C:2]([CH3:15])([CH3:3])[C:4](=[N:13][OH:14])[CH2:5][O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1参加物
4
実験手順
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.).
後処理
- temperaturewas heated
- temperatureto reflux
- dissolutiondissolved (2 hours)
- filtrationFiltration and evaporation of solvent
- customgave a brown solid, which
- washby washing with benzene
- customRecrystallisation from isopropanol (a small inorganic residue
出典と根拠
- ORDレコード
- ord-5612de6111174038b10c2041d6f52e8b
- 出典データセット
- uspto-grants-1979_05
- 特許番号
- US04156725
反応ノート
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