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Hydrochloric Acid → Ethyl 4-(3,4-dichlorophenyl)-2,4-dioxobutanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Diethyl Oxalate | HCID 7268 | — |
| 反応物 | Ethanone, 1-(3,4-dichlorophenyl)- | HCID 75841 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | Ethyl 4-(3,4-dichlorophenyl)-2,4-dioxobutanoate | HCID 10017017 | — |
反応手順
To a solution of t-BuOK (0.05 mol, 5.6 g) in benzene (200 mL) was added dropwise a benzene (50 mL) solution of 3,4-dichloroacetophenone 5.1 (0.05 mol, 9.45 g) and diethyloxalate (0.055 mol, 8.1 g). The resultant mixture was stirred for 8 h at room temperature, then 10% aqueous HCl solution (100 mL) was added to the mixture. The organic layer was separated and washed with brine, dried over sodium sulfate and concentrated in vacuo. The crude product was purified by column chromatography using dichloromethane as eluent to yield the title compound. Yield: 7.5 g (52%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08871761B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-1934ae3a8e0442dda759df426fd55823 |
| 出典メモ | uspto-grants-2014_10 |