関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Triphenylsulfonium Bromide | HCID 11984010 | — |
| 反応物 | 2,2-Difluoro-3-(methacryloyloxy)pentanoic acid | HCID 58413440 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | Triphenylsulfonium 2,2-difluoro-3-methacryloyloxypentanoate | HCID 86657208 | 101.1% |
反応手順
A 1-L glass flask equipped with a dropping funnel was charged with 108 g (0.486 mol) of 1-hydroxycarbonyl-1,1-difluoro-2-butyl methacrylate and 108 g of chloroform, which were stirred and cooled at 0° C. Then 224 g (0.560 mol/1.15 equivalent) of a 10 wt % sodium hydroxide aqueous solution was added dropwise to the solution, which was stirred at room temperature for 1 hour. Then 169 g (0.492 mol/1.01 equivalent) of triphenylsulfonium bromide in 432 g of chloroform was added to the solution, which was stirred at room temperature for 1 hour. After the completion of reaction was confirmed by 1H-NMR spectroscopy, an organic layer was separated from the reaction liquid and washed 3 times with 300 g of water. The organic layer was concentrated in vacuum, obtaining 238 g (yield 81%, purity 80%) of triphenylsulfonium 2,2-difluoro-3-methacryloyloxypentanoate, designated Monomer Z-1, having the following structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08632939B2 |
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| 出典データセット | uspto-grants-2014_01 |
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| ORD ID | ord-3df02a539c1841cd823538d1d63b62a2 |
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| 出典メモ | uspto-grants-2014_01 |
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