関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Pivaloyl chloride | HCID 62493 | — |
| 反応物 | 4-Chloro-2-fluorotoluene | HCID 520630 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-(3-Fluoro-4-methylphenyl)-1-trimethylacetyl-1,4-dihydropyridine | HCID 14851973 | — |
反応手順
To a solution of 45 ml pyridine in 800 ml tetrahydrofuran (THF) was added dropwise 50 ml trimethylacetyl chloride. The mixture was stirred 3 hrs. at room temperature, 4.0 g cuprous iodide was added, and the mixture stirred for 1 hr. longer. The mixture was then cooled to -40° C. and a Grignard reagent prepared from 45 ml 2-fluoro-4-chlorotoluene and 10 g magnesium in 300 ml THF was added dropwise The reaction mixture was stirred overnight at room temperature, ammonium chloride solution added, and the product was extracted and isolated to give 90 g of an oil used directly in the next reaction.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04959363 |
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| 出典データセット | uspto-grants-1990_09 |
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| ORD ID | ord-597cc87d81364b66a4448ffc9aee34c3 |
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| 出典メモ | uspto-grants-1990_09 |
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