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 | Oct-7-yn-1-yl 4-methylbenzene-1-sulfonate | HCID 10779145 | — |
| 反応物 | 2-(3,3,3-Trifluoropropylsulfonyl)acetonitrile | HCID 57425671 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 2-(3,3,3-Trifluoropropylsulfonyl)-9-decynenitrile | HCID 86642986 | 26% |
反応手順
To a solution of 1.0 g of 7-octynyl p-toluenesulfonate and 0.7 g of (3,3,3-trifluoropropylsulfonyl)acetonitrile in 30 ml of dimethyl sulfoxide was added 0.5 g of potassium carbonate at room temperature. The reaction mixture was stirred at room temperature for 2 hours, at 60° C. for 2 hours, and then at 90° C. for 6 hours. The reaction mixture was allowed to stand to cool to nearly room temperature. 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 0.28 g of 2-(3,3,3-trifluoropropylsulfonyl)-9-decynenitrile (hereinafter referred to as the present compound (25)).
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-7cf2a36cffb54379bc2be9cc2145193d |
|---|
| 出典メモ | uspto-grants-2012_08 |
|---|