関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Silane, tris(1-methylethyl)- | HCID 138754 | — |
| 反応物 | 2,3,3,3-Tetrafluoro-2-(heptafluoropropoxy)propanoyl chloride | HCID 2782597 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 生成物 | CF3CF2CF2Ocf(CF3)cho | HCID 15717421 | 53.5% |
反応手順
A 3-necked round bottom flask equipped with a dropping funnel and reflux condenser was charged with 10% Pd/C(0.35 g) and cooled to 0° C. Triisopropylsilane (6.0 g) was added. CF3CF2CF2OCF(CF3)COCl (10.9 g) was added, and the mixture was stirred at 25° C. for 75 hr. During this period, a total of 0.5 g of additional catalyst was added in ca. 0.1 g increments. Vacuum transfer and separation of the lower layer after chilling at -25° C. provided 5.26 g of liquid. 1H NMR (THF-d8 /F11): 9.9 (m). 19F NMR: -79.4 (m), -81.1 (s), -81.4 (t, J=7.2), -129.5 (s), -138.8 (m). 1H-decoupling experiment showed JHCCFCa. 2.5 Hz.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05414140 |
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| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-1c4d85ecbe5f4908925f4e153def61fc |
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| 出典メモ | uspto-grants-1995_05 |
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