Sodium Carbonate → N-(4,4-dimethylcyclohexylidene)hydroxylamine
反応式
[CH3:1][C:2]1([CH3:9])[CH2:7][CH2:6][C:5](=O)[CH2:4][CH2:3]1.[NH2:10][OH:11].Cl.C([O-])([O-])=O.[Na+].[Na+]>O.C(O)C>[CH3:1][C:2]1([CH3:9])[CH2:7][CH2:6][C:5](=[N:10][OH:11])[CH2:4][CH2:3]1参加物
6
実験手順
To 4,4-Dimethylcyclohexanone (50 g, 396.19 mmol), NH2OH.HCl (35.84 g, 515.75 mmol) in H2O (190 mL) and ethanol (250 mL) was added a solution of Na2CO3 (54.16 g, 510.99 mmol) in water (170 mL) dropwise over a period of 20 minutes. After complete addition, reaction mixture was heated to reflux for 3h. The ethanol was evaporated, and the residue extracted into ethyl acetate (4×120 mL). The combined organic layer was washed with water (150 mL), brine (150 mL) and dried over sodium sulfate and concentrated to afford 45 g (80.4%) 4,4-dimethyl cyclohexanone oxime (I 6a) as white solid.
後処理
- additionAfter complete addition, reaction mixture
- temperaturewas heated
- temperatureto reflux for 3h
- customThe ethanol was evaporated
- extractionthe residue extracted into ethyl acetate (4×120 mL)
- washThe combined organic layer was washed with water (150 mL), brine (150 mL)
- dry with materialdried over sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-e03278eef4564eb4a7b51ecd215cd9c5
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09447039B2
反応ノート
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