関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Chlorosulfonic acid | HCID 24638 | — |
| 反応物 | 1,1,3,3,3-Pentafluoropropene | HCID 69647 | — |
| 生成物 | Ethyl 3,3,3-Trifluoropropionate | HCID 2782349 | 87% |
反応手順
A 100 mL Hastelloy shaker tube was loaded with 26.5 g (0.227 mole) chlorosulfuric acid, cooled in liquid nitrogen, evacuated and loaded with 30 g (0.225 mole) of 1,1,3,3,3-pentafluoropropene. The reaction vessel was allowed to warm and kept on a shaker at 40° C. at autogenous pressure for 6 hours. The pressure tube was unloaded, and the reaction mixture was added drop by drop into the flask containing 60 ml of ethanol at −10° C. over a 15 minute period. The reaction mixture was stirred overnight at 20° C. and then was poured into 200 ml of ice water. The organic layer was separated, washed with sodium bicarbonate, water, and dried under MgSO4. Distillation gave 31 g of CF3CH2COOEt (87%), bp 108-109° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07728183B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-41cf697fc97a4e12acff528e5f786692 |
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| 出典メモ | uspto-grants-2010_06 |
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