関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Diethyl Malonate | HCID 7761 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Bromo-3-fluorotoluene | HCID 573280 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Diethyl (2-fluoro-4-methylphenyl)malonate | HCID 17974023 | 59.6% |
反応手順
0.49 mol of diethyl malonate was added at 60° C. inside 2 hours to a mixture of 0.51 mol of NaH and 140 ml of 1,4-dioxane. The mixture was stirred for approximately 10 min at 60° C. and then 0.05 mol of Cu(I)Br was added. After 15 min, a mixture of 0.25 mol of 4-bromo-3-fluorotoluene and 10 ml of 1,4-dioxane was added. The reaction mixture was heated at 100° C. for approximately 15 hours and was then cooled to 15° C. After acidifying with 35 ml of 12N HCl at 15 to 20° C., the precipitate produced was filtered off. The filtrate was extracted and the organic phases, after separation, were dried and then freed from the solvent. 40 g of the title compound were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07094894B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-040a36dbcef644d3b7a53d23ebd88f75 |
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| 出典メモ | uspto-grants-2006_08 |
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