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Diethyl Ether → 3-(2,4-Dichloro-5-fluorophenyl)-3-oxopropanenitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Benzoic acid, 2,4-dichloro-5-fluoro-, ethyl ester | HCID 13630722 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-(2,4-Dichloro-5-fluorophenyl)-3-oxopropanenitrile | HCID 13630721 | 34.5% |
反応手順
A mixture of 47.4 g of ethyl 2,4-dichloro-5-fluoro-benzoate and 8.2 g of anhydrous acetonitrile are added dropwise to a suspension of 6.1 g of 80% strength sodium hydride in 100 ml of anhydrous tetrahydrofuran under reflux in the course of about 1 hour. The mixture is heated at the boiling point under reflux for a further hour and cooled to room temperature, and 150 ml of ether are added. The precipitate is filtered off with suction and dissolved in 50 ml of ice-water and the solution is acidified to pH=6 with 10% strength hydrochloric acid. The precipitate is filtered off cold with suction, rinsed with ice-water and dried in vacuo at 40° C. 16 g of 2,4-dichloro-5-fluoro-benzoylacetonitrile of melting point 96°-98° C. are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04914228 |
| 出典データセット | uspto-grants-1990_04 |
| ORD ID | ord-3c6183603a3443ac969e7cc9309cc47c |
| 出典メモ | uspto-grants-1990_04 |