反応式
[CH3:1][C:2]1[N:7]=[C:6]([O:8][CH2:9][C:10]2[CH:17]=[CH:16][C:13]([CH:14]=O)=[CH:12][CH:11]=2)[CH:5]=[CH:4][CH:3]=1.[N+:18]([CH3:21])([O-:20])=[O:19].C([O-])(=O)C.[NH4+]>C(O)(=O)C>[CH3:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]([O:8][CH2:9][C:10]2[CH:17]=[CH:16][C:13](/[CH:14]=[CH:21]/[N+:18]([O-:20])=[O:19])=[CH:12][CH:11]=2)[N:7]=1参加物
5
反応条件
- 温度
- 110 °C
実験手順
To a solution of 4-(6-methyl-pyridin-2-yloxymethyl)-benzaldehyde (4.19 g, 18.5 mmol) described in Manufacturing Example 3-1-2 in acetic acid (30 mL) were added nitromethane (5.65 g, 92.6 mmol) and ammonium acetate (2.85 g, 37.0 mmol) under nitrogen atmosphere, which was stirred for 3 hours at 110° C. The reaction mixture was partitioned into water and ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under a reduced pressure to obtain the title compound (5.50 g) as a crude product.
後処理
- customThe reaction mixture was partitioned into water and ethyl acetate
- washThe organic layer was washed with water and saturated aqueous sodium chloride
- dry with materialdried over anhydrous magnesium sulfate
- customthe solvent was evaporated under a reduced pressure
出典と根拠
- ORDレコード
- ord-8d3d40763f0c4de1a07f9332ef3d77f1
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08841327B2
関連ノート
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