関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Decafluorobiphenyl | HCID 67949 | — |
| 反応物 | Potassium | HCID 5462222 | — |
| 反応物 | HCID 23672351 | HCID 23672351 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(4-Benzyloxycarbonylphenoxy)nonafluorobiphenyl | HCID 10875244 | 92% |
反応手順
37.4 g of decafluorobiphenyl (0.112 mol) are dissolved in 700 ml of dimethylformamide, the mixture is cooled to −10° C. using a cryostat, and a solution of 29.8 g of potassium 4-benzyloxycarbonylphenoxide (0.112mol) in 300 ml of dimethylformamide is then added dropwise over the course of 2 hours. After 48 hours at −10° C., the potassium salt has reacted. The dimethylformamide is then removed in a rotary evaporator, the residue is taken up in a little tetrahydrofuran, and the solution is filtered through a silica-gel column. The clear solution obtained is evaporated in a rotary evaporator until a white solid precipitates out. The solid is then stirred in n-hexane, filtered off using a fluted filter and then dried for 48 hours under nitrogen at 40° C./10 mbar in a vacuum drying cabinet (yield: 92%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06310238B1 |
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| 出典データセット | uspto-grants-2001_10 |
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| ORD ID | ord-5755cd6649ba4362b9da2de0783343fc |
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| 出典メモ | uspto-grants-2001_10 |
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