Veratraldehyde → N-[(3,4-Dimethoxyphenyl)methylidene]hydroxylamine
反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[CH:6]=O.[NH2:13][OH:14].Cl.C([O-])([O-])=O.[Na+].[Na+]>C(O)C.O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:6]=[N:13][OH:14])[CH:8]=[CH:9][C:10]=1[O:11][CH3:12]参加物
5
実験手順
After dissolving 3,4-dimethoxybenzaldehyde (1.00 g, 0.081 mmol) in 60 mL of ethyl alcohol/water (1/1, v/v) solution, H2NOH HCl (0.54 g, 7.823 mmol) was added. While stirring the reaction mixture, Na2CO3 (0.83 g, 7.823 mmol) was added slowly at below 0° C. The reaction was continued for 1 hr in an oil bath preheated to 60-65° C. After the reaction was completed, 1.05 g (96.4%) of the target product was obtained by extracting with ethyl acetate, drying over anhydrous MgSO4 and removing the solvent under reduced pressure.
後処理
- additionwas added slowly at below 0° C
- custompreheated to 60-65° C
出典と根拠
- ORDレコード
- ord-6a098c5249ff4df9a1180c5efc6c3211
- 出典データセット
- uspto-grants-2004_01
- 特許番号
- US06673800B2
反応ノート
読み込み中…