関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4,4,4-Trifluoro-2-butenyl p-toluenesulfonate | HCID 53655839 | — |
| 反応物 | 2-(3,3,3-Trifluoropropylsulfonyl)propionitrile | HCID 57788363 | — |
| 生成物 | 6,6,6-Trifluoro-2-methyl-2-(3,3,3-trifluoropropylsulfonyl)-4-hexenenitrile | HCID 72281791 | — |
反応手順
To a solution of 1.5 g of 4,4,4-trifluoro-2-butenyl p-toluenesulfonate and 1.2 g of 2-(3,3,3-trifluoropropylsulfonyl)propionitrile in 30 ml of tetrahydrofuran was added 0.2 g of sodium hydride (60% in oil) at room temperature. The reaction mixture was stirred at the same temperature for 2 days. To the reaction mixture was added 10% hydrochloric acid and then extracted with ethyl acetate. The organic layer was washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The obtained residue was subjected to silica gel chromatography to obtain 0.80 g of 6,6,6-trifluoro-2-methyl-2-(3,3,3-trifluoropropylsulfonyl)-4-hexenenitrile (hereinafter referred to as the present compound (34)).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08247595B2 |
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| 出典データセット | uspto-grants-2012_08 |
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| ORD ID | ord-4fb3e7227b194dea95a8f344ba55403c |
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| 出典メモ | uspto-grants-2012_08 |
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