反応式
[C:1]1([CH2:7][C:8]#[N:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P([O-])(OCC)(SCC)=[S:11]>Cl.C(OCC)(=O)C>[C:1]1([CH2:7][C:8]([NH2:9])=[S:11])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1参加物
4
実験手順
A solution of phenylacetonitrile (10.0 g, 85.4 mmol) and diethyl dithiophosphate (17.5 g, 93.9 mmol) in 4N-HCl/ethyl acetate (400 mL) was stirred at room temperature for 16 hours. This reaction mixture was washed with water and saturated aqueous sodium hydrogen carbonate solution, dried over MgSO4, filtered, and concentrated under reduced pressure. The residue was crystallized from ethanol to provide 7.1 g of the title compound. Yield 55%.
後処理
- washThis reaction mixture was washed with water and saturated aqueous sodium hydrogen carbonate solution
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe residue was crystallized from ethanol
出典と根拠
- ORDレコード
- ord-b95e9b3ac9114e76baa3b07b56de8fcd
- 出典データセット
- uspto-grants-2001_06
- 特許番号
- US06248766B1
関連ノート
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