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Hydrochloric Acid → Methyl 6,6,6-trifluoro-2-(3,3,3-trifluoropropylsulfonyl)-4-hexenoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4,4,4-Trifluoro-2-butenyl p-toluenesulfonate | HCID 53655839 | — |
| 反応物 | Methyl 2-(3,3,3-trifluoropropylsulfonyl)acetate | HCID 57425720 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | Methyl 6,6,6-trifluoro-2-(3,3,3-trifluoropropylsulfonyl)-4-hexenoate | HCID 86642981 | 47.9% |
反応手順
To a solution of 2.4 g of 4,4,4-trifluoro-2-butenyl p-toluenesulfonate and 2.0 g of methyl (3,3,3-trifluoropropylsulfonyl)acetate in 50 ml of dimethyl sulfoxide, 1.2 g of potassium carbonate was added at room temperature and stirred at the same temperature for 16 hours. To the reaction mixture, 10% hydrochloric acid was added, followed by extraction 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 1.40 g of methyl 6,6,6-trifluoro-2-(3,3,3-trifluoropropylsulfonyl)-4-hexenoate (hereinafter referred to as the present compound (17)).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08247595B2 |
| 出典データセット | uspto-grants-2012_08 |
| ORD ID | ord-f9a5c1b7fdfc49adb3b8f2411ba41995 |
| 出典メモ | uspto-grants-2012_08 |