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Hydrochloric Acid → Diethyl 2-(4-methoxyphenyl)malonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Diethyl Carbonate | HCID 7766 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Ethyl 4-methoxyphenylacetate | HCID 84174 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Diethyl 2-(4-methoxyphenyl)malonate | HCID 2785178 | — |
反応手順
27.7 g of ethyl 4-methoxyphenylacetate and 34 ml of diethyl carbonate were dissolved in 150 ml of N,N-dimethylformamide, and the solution was subjected to reflux under heating, while gradually adding 6.5 g of sodium hydride for 1 hour. After further refluxing under heating for 2 hours, the resulting reaction solution was poured into a mixture of ice water and hydrochloric acid, followed by extraction with ethyl acetate. The resulting organic layer was washed with water, and then dried to distill off the solvent. The residue thus obtained was purified by silica gel column chromatography using toluene as an eluant, thereby obtaining 26.7 g of ethyl 2-ethoxycarbonyl-2-(4-methoxyphenyl)acetate in the form of light yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05962695 |
| 出典データセット | uspto-grants-1999_10 |
| ORD ID | ord-cb7c7149100642379d1d2ffb3672023e |
| 出典メモ | uspto-grants-1999_10 |