反応式
[C:1](#[N:3])[CH3:2].[Li]CCCC.[Cl:9][C:10]1[CH:18]=[C:17]([Cl:19])[CH:16]=[CH:15][C:11]=1[C:12](Cl)=[O:13]>C1COCC1>[Cl:9][C:10]1[CH:18]=[C:17]([Cl:19])[CH:16]=[CH:15][C:11]=1[C:12](=[O:13])[CH2:2][C:1]#[N:3]参加物
5
実験手順
To a stirred solution of acetonitrile (2.0 mL, 38.2 mmol) in THF (50 mL) at −78° C. was added nBuLi (1.81 M in hexane, 16 mL, 28.7 mmol). The resulting slurry was kept at −78° C. for 15 min and 2,4-dichlorobenzoyl chloride (2.0 g, 9.55 mmol) was added dropwise to the acetonitrile anion. After 40 min, the reaction was quenched by addition of saturated NH4Cl (30 mL). THF was removed under reduced pressure and the suspension was filtered. The solid was washed with H2O (100 mL) and dried to give 3-(2,4-dichlorophenyl)-3-oxopropanenitrile (2.0 g, 98%, >95% purity) as a light yellow solid.
後処理
- waitAfter 40 min
- customthe reaction was quenched by addition of saturated NH4Cl (30 mL)
- customTHF was removed under reduced pressure
- filtrationthe suspension was filtered
- washThe solid was washed with H2O (100 mL)
- customdried
出典と根拠
- ORDレコード
- ord-944f8150ba9f49919021ddc8a8e53b70
- 出典データセット
- uspto-grants-2009_09
- 特許番号
- US07589088B2
関連ノート
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