関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2,5-Difluorobenzophenone | HCID 522826 | — |
| 反応物 | Dilithium Sulfide | HCID 10290727 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Fluoro-2-benzoylthiophenol | HCID 23074232 | 98% |
反応手順
To a solution of 10.1 g of 2,5-difluorobenzophenone in 200 ml of DMSO was added 3.5 g of lithium sulfide (manufactured by ALDRICH CHEMICAL COMPANY) and the mixture was stirred in a nitrogen atmosphere at 120° C. for 3 hours. To the reaction solution was added 200 ml of 1N hydrochloric acid under ice cooling, and further 400 ml of ethyl acetate and 200 ml of water were added to the mixture to separate it. The organic layer was washed with 400 ml of water and then with 200 ml of saturated saline. The organic layer was dried over anhydrous sodium sulfate and then concentrated to obtain 10.54 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07803792B2 |
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| 出典データセット | uspto-grants-2010_09 |
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| ORD ID | ord-15fed540865d4c7ea9b9da66f2fe5595 |
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| 出典メモ | uspto-grants-2010_09 |
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