反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:12]=[CH:13][C:14]=1[Cl:15])[CH2:5][NH:6][C:7](=[O:11])[CH2:8][C:9]#[N:10].CO[CH:18]=[CH:19][C:20](=O)[CH3:21].N12CCN(CC1)CC2>COCCO>[Cl:1][C:2]1[CH:3]=[C:4]([CH:12]=[CH:13][C:14]=1[Cl:15])[CH2:5][N:6]1[C:20]([CH3:21])=[CH:19][CH:18]=[C:8]([C:9]#[N:10])[C:7]1=[O:11]参加物
5
実験手順
A solution of 49.7 g. (0.204 mole) of N-(3,4-dichlorobenzyl)-2-cyanoacetamide, 48.0 g. (0.48 mole) of 4-methoxy-3-buten-2-one, and 4 g. of 1,4-diazabicyclo (2.2.2) octane (DABCO) in 160 ml. of 2-methoxyethanol is refluxed for 4 hr. The dark reaction mixture is then concentrated in vacuo and the crude solid is isolated by filtration from the resulting slurry and washed with ether. The crude product is dissolved in methylene chloride and the organic solution is washed with water, 2N-HCl and finally with more water. The methylene chloride is removed and the product is obtained in 62% yield by ether trituration.
後処理
- customThe dark reaction mixture
- concentrationis then concentrated in vacuo
- customthe crude solid is isolated by filtration from the resulting slurry
- washwashed with ether
- dissolutionThe crude product is dissolved in methylene chloride
- washthe organic solution is washed with water, 2N-HCl and finally with more water
- customThe methylene chloride is removed
- customthe product is obtained in 62% yield by ether trituration
出典と根拠
- ORDレコード
- ord-8676f4fd4901411d9d023b915b59605f
- 出典データセット
- uspto-grants-1977_06
- 特許番号
- US04028084
関連ノート
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