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P-Chloroacetophenone → Ethyl 3-(4-chlorophenyl)-3-oxopropanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | P-Chloroacetophenone | HCID 7467 | — |
| 反応物 | Diethyl Carbonate | HCID 7766 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 生成物 | Ethyl 3-(4-chlorophenyl)-3-oxopropanoate | HCID 101336 | — |
反応手順
The starting material is prepared as follows: A solution of 96.6 g of 4-chloro acetophenone in 300 ml of diethyl carbonate is added dropwise to a suspension of 34 g sodium hydride (55% in mineral oil, washed twice with diethyl ether) in 400 ml of diethyl carbonate at ice bath temperature, then at room temperature for 2 days. To the dark solution is then added crushed ice and 5N hydrochloric acid to adjust the pH to 6-7. After dilution with diethyl ether, the layers are separated, the organic phase washed with a saturated aqueous sodium chloride solution and then dried over anhydrous sodium sulfate. After removal of the solvents, the oily ethyl 3-(4-chloro-phenyl)-3-oxo-propionate is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04028381 |
| 出典データセット | uspto-grants-1977_06 |
| ORD ID | ord-59fd556cd5d4406f8786802ef4bbe8d5 |
| 出典メモ | uspto-grants-1977_06 |