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Ethanol → Ethyl (2-chlorobenzoyl)acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Diethyl Carbonate | HCID 7766 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Ethanone, 1-(2-chlorophenyl)- | HCID 72864 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ethyl (2-chlorobenzoyl)acetate | HCID 292405 | — |
反応手順
Sodium hydride (8.7 grams) and 21.4 grams of diethyl carbonate are suspended in 100 ml of tetrahydrofuran, 14 grams of o-chloroacetophenone is gradually dropped thereinto by keeping the inner temperature at 40° to 50° C., then a small amount of ethanol is added thereto and heated to reflux for four hours. After cooling, 20 ml of ethanol is added thereto, the mixture is poured into ice water, and extracted with ether. Ether extracts are combined, washed with water, dried with anhydrous magnesium sulfate, and ether is evaporated therefrom. The resulting oil is purified by distillation in vacuo to give 8.8 grams of colorless, oily product, b.p. 120° to 125° C./1 mmg Hg.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04711898 |
| 出典データセット | uspto-grants-1987_12 |
| ORD ID | ord-3823c647e0a742aa85112ba7366a48a0 |
| 出典メモ | uspto-grants-1987_12 |