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-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.).
後処理
- temperaturewas heated
- dissolutiondissolved (3.5 h)
- filtrationFiltration and removal of solvents
- customgave an off-white solid, which
- washby washing with benzene
- customTwo recrystallisations from isopropanol (a small inorganic residue
出典と根拠
- ORDレコード
- ord-65e01234b61e4059b2ef6ebce0ad46a8
- 出典データセット
- uspto-grants-1976_01
- 特許番号
- US03933820
反応ノート
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