化工社化工社 化学情報印刷レポート · 研究参考用
Acetonitrile → 3-(2,4-Dichlorophenyl)-3-oxopropanenitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | 2,4-Dichlorobenzoyl chloride | HCID 66645 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-(2,4-Dichlorophenyl)-3-oxopropanenitrile | HCID 13630728 | 97.8% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07589088B2 |
| 出典データセット | uspto-grants-2009_09 |
| ORD ID | ord-944f8150ba9f49919021ddc8a8e53b70 |
| 出典メモ | uspto-grants-2009_09 |