関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1,4-Dibromo-1,1,2,2-tetrafluorobutane | HCID 87719 | — |
| 反応物 | Methyl 2-(3,3,3-trifluoropropylsulfonyl)acetate | HCID 57425720 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | Methyl 6-bromo-5,5,6,6-tetrafluoro-2-(3,3,3-trifluoropropylsulfonyl)hexanoate | HCID 59370910 | 27.2% |
反応手順
To a solution of 1.2 g of 1,4-dibromo-1,1,2,2-tetrafluorobutane and 1.0 g of methyl (3,3,3-trifluoropropylsulfonyl)acetate in 30 ml of dimethyl sulfoxide was added 0.2 g of sodium hydride (60% in oil) at room temperature. The mixture was stirred at the same temperature for 3 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 0.50 g of methyl 6-bromo-5,5,6,6-tetrafluoro-2-(3,3,3-trifluoropropylsulfonyl)hexanoate (hereinafter referred to as the present compound (4)).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08158829B2 |
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| 出典データセット | uspto-grants-2012_04 |
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| ORD ID | ord-0940b8c9ec2a4bc481aa1c46454dd26c |
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| 出典メモ | uspto-grants-2012_04 |
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