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 | HCID 178447996 | HCID 178447996 | — |
| 生成物 | HCID 178447998 | HCID 178447998 | 60% |
反応手順
Then, a mixed solution containing 1.3 g (6.31 mmol) of 2-(trans-4-n-propylcyclohexyl)-1,1,2-trifluoroethylene obtained in Example 1 and 10 ml of dry THF, was dropwise added thereto at the same temperature over a period of 15 minutes. The mixture was reacted at the same temperature for one hour and then the temperature was raised to -10° C. Then, 100 ml of 1N hydrochloric acid was added thereto. The organic layer was separated. The aqueous layer was extracted with n-hexane, and the extract was combined with the organic layer. The combined organic layer was washed with water and dried. Then, the solvent was distilled off, and the obtained crude solution was purified by silica gel column chromatography. The obtained solid was further recrystallized from ethanol to obtain 1.18 g (yield: 60%) of (E)-1,2-bis(trans-4-n-propylcyclohexyl)-1,2-difluoroethylene.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05621147 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-1564235662c9419a825d50edec702130 |
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| 出典メモ | uspto-grants-1997_04 |
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