関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 4-Iodopyridine | HCID 609492 | — |
| 反応物 | (3,3,3-Trifluoroprop-1-en-2-yl)boronic acid | HCID 2782677 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 4-[1-(Trifluoromethyl)ethenyl]pyridine | HCID 59570355 | 73.5% |
反応手順
To 1,4-dioxane were added 3.22 g of 4-iodopyridine, 10.87 g of potassium carbonate, 0.036 g of tetrakis(triphenylphosphinepalladium) and 5.5 g of 1-(trifluoromethyl)vinylboronic acid, and the mixture was stirred at 110° C. for 8 hours. Thereafter, this solution was poured into an aqueous saturated ammonium chloride solution, followed by extraction with diethyl ether three times. The organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 2.0 g of 4-[1-(trifluoromethyl)ethenyl]pyridine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08318776B2 |
|---|
| 出典データセット | uspto-grants-2012_11 |
|---|
| ORD ID | ord-9f0c2151f2b44a58a621a8a51def4c6e |
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| 出典メモ | uspto-grants-2012_11 |
|---|
