Acetonitrile → HCID 21794538、化合物
反応式
[OH:1][C:2]1[CH:9]=[C:8]([O:10][CH3:11])[CH:7]=[CH:6][C:3]=1[CH:4]=[O:5].C(=O)([O-])[O-].[K+].[K+].Br[CH2:19][C:20]#[N:21].C(#N)C>O>[CH:4]([C:3]1[CH:6]=[CH:7][C:8]([O:10][CH3:11])=[CH:9][C:2]=1[O:1][CH2:19][C:20]#[N:21])=[O:5]参加物
6
実験手順
The mixture of 2-hydroxy-4-methoxybenzaldehyde (9.50 g), potassium carbonate (17.3 g), bromoacetonitrile (11.2 g) and acetonitrile (100 ml) was stirred at room temperature for 12 hours. Water was added to the reaction mixture, which was extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous sodium chloride solution, then dried and concentrated. The residue was purified by alumina column chromatography (eluent: ethyl acetate), and then recrystallized from ethyl acetate-hexane to obtain the entitled compound (10.7 g).
後処理
- extractionwas extracted with ethyl acetate
- washThe organic layer was washed with water
- dry with materiala saturated aqueous sodium chloride solution, then dried
- concentrationconcentrated
- customThe residue was purified by alumina column chromatography (eluent: ethyl acetate)
- customrecrystallized from ethyl acetate-hexane
出典と根拠
- ORDレコード
- ord-481ef0b581d6449c9e54b2589a22d346
- 出典データセット
- uspto-grants-2001_12
- 特許番号
- US06329389B1
反応ノート
読み込み中…