関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Vinylbenzoyl chloride | HCID 11052028 | — |
| 反応物 | HCID 86612198 | HCID 86612198 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 86639514 | HCID 86639514 | — |
反応手順
Under ice cooling, 2.0 g (12 mmol) of the resulting 4-vinylbenzoyl chloride in methylene chloride was added dropwise to a mixture of 4.9 g (10 mmol) of triphenylsulfonium 2-hydroxy-1,1,3,3,3-pentafluoropropane-1-sulfonate in Synthesis Example 1-11, 1.21 g (12 mmol) of triethylamine, 0.24 g (2 mmol) of N,N-dimethylaminopyridine, and 20 g of methylene chloride. The reaction mixture was stirred at room temperature for 2 hours. Thereafter, 11 g of 5% dilute hydrochloric acid was added. The organic layer was separated and washed with water whereupon methylene chloride was distilled off under vacuum. The residue was combined with 30 g of methyl isobutyl ketone and washed with dilute aqueous ammonia and then with water, whereupon the methyl isobutyl ketone was distilled off under vacuum. Diisopropyl ether was added to the residue, followed by decantation. The target compound, triphenylsulfonium 1,1,3,3,3-pentafluoro-2-(4-vinyl-benzoyloxy)-propane-1-sulfonate was obtained as colorless oil (5.3 g, yield 85%). The compound has the following structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08057985B2 |
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| 出典データセット | uspto-grants-2011_11 |
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| ORD ID | ord-0a62daba88754b8f907e8fdc4f623115 |
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| 出典メモ | uspto-grants-2011_11 |
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