関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Diethyl Oxalate | HCID 7268 | — |
| 反応物 | Ethyl ethoxyacetate | HCID 69955 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | HCID 11138994 | HCID 11138994 | 90% |
反応手順
A stirred mixture of molten sodium metal (24.15 g, 1.05 mol) in toluene is treated with ethanol (55.2 g, 1.2 mol) over a 1 hr period at 100° C.-110° C., heated at reflux temperatures for 0.5 hr, cooled to 30° C., treated with diethyl oxalate (160.6 g, 1.1 mol) over a 10 min period at 30° C.-45° C., treated with ethyl ethoxyacetate (132 g, 98%, 0.98 mol) over an 0.5 hr period at 45° C.-50° C., heated at 55° C.-60° C. for 1.5 hr and poured into 328 g of 14% HCl with cooling. The resultant mixture is separated. The title product is obtained in the organic phase as a 40.9% solution, identified by HRGC analysis, total yield is 204.2 g (90% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05925764 |
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| 出典データセット | uspto-grants-1999_07 |
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| ORD ID | ord-515f3a087fd6457cbc7a1a3059eb1a52 |
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| 出典メモ | uspto-grants-1999_07 |
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