関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,1,2,2-Tetrafluoroethyl iodide | HCID 136180 | — |
| 反応物 | HCID 178506332 | HCID 178506332 | — |
| 触媒 | Copper | HCID 23978 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-pentafluoroethyl-4-(1,1,2,2-tetrafluoroethyl)-1H-pyrazole | HCID 178506047 | 10.5% |
反応手順
4-Iodo-3-pentafluoroethyl-1H-pyrazole (6.24 g), copper powder (3.81 g), Iodo-1,1,2,2-tetrafluoroethane (9.12 g) and DMF (30 ml) were set in an autoclave and heated and stirred for 8 hours, maintaining the inside temperature of 120-125° C. After cooling to room temperature, the insoluble material was filtered off through Celite and washed with diethyl ether. The filtrate was diluted with water and extracted with diethyl ether. The organic phase was washed with water and dried over sodium sulfate, and concentrated under the reduced pressure. The crude product was distilled under reduced pressure to obtain 3-pentafluoroethyl-4-(1,1,2,2-tetrafluoroethyl)-1H-pyrazole (0.60 g), bp. 125-135° C./20 mbar.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07674807B2 |
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| 出典データセット | uspto-grants-2010_03 |
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| ORD ID | ord-e2f53f7ccd934c58b63d46216c3a8ae5 |
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| 出典メモ | uspto-grants-2010_03 |
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