反応式
[CH2:1]([O:3][P:4]([CH:6]([O:10][CH2:11][CH3:12])[O:7][CH2:8][CH3:9])[O-:5])[CH3:2].[C:13](#[N:17])[C:14]([CH3:16])=[CH2:15].[H-].[Na+].C(O)(=O)C>C(O)C>[CH2:1]([O:3][P:4]([CH2:15][CH:14]([C:13]#[N:17])[CH3:16])([CH:6]([O:10][CH2:11][CH3:12])[O:7][CH2:8][CH3:9])=[O:5])[CH3:2]参加物
実験手順
The starting material may be prepared as follows: A solution of 23.5 g of ethyl(diethoxymethyl)phosphonite and 6.7 g of methacrylonitrile in 30 ml of ethanol is added dropwise to a stirred mixture of 1.2 g of sodium hydride (50% dispersion in oil) in 30 ml of ethanol at 0° C. under an atmosphere of nitrogen. The reaction mixture is allowed to warm to room temperature and stirred for 4 hours. 1 ml of glacial acetic acid is added and the mixture is concentrated under reduced pressure. The resulting crude product is dissolved in 50 ml of ethyl acetate, washed twice with 25 ml of water, and the organic extract is dried over magnesium sulphate, and then concentrated under reduced pressure. The crude product is distilled under reduced pressure to give ethyl-2-cyanopropyl(diethoxymethyl)phosphinate, b.p. 116° C./0.01 mbar, 31P=+40.4 and +40.3 ppm (CDCl3).
後処理
- customThe starting material may be prepared
- concentrationthe mixture is concentrated under reduced pressure
- dissolutionThe resulting crude product is dissolved in 50 ml of ethyl acetate
- washwashed twice with 25 ml of water
- extractionthe organic extract
- dry with materialis dried over magnesium sulphate
- concentrationconcentrated under reduced pressure
- distillationThe crude product is distilled under reduced pressure
出典と根拠
- ORDレコード
- ord-bb9103e32fe2431a91d4f1cf01b957d5
- 出典データセット
- uspto-grants-1987_04
- 特許番号
- US04656298
関連ノート
読み込み中…