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Diphenyl sulfoxide → Diphenyl(5,7-diethylthioxanthene-9-one-2-yl)sulfonium trifluoromethanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diphenyl sulfoxide | HCID 13679 | — |
| 反応物 | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| 反応物 | 2,4-Diethylthioxanthone | HCID 122825 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Diphenyl(5,7-diethylthioxanthene-9-one-2-yl)sulfonium trifluoromethanesulfonate | HCID 23054201 | 64% |
反応手順
To 320 ml of dichloromethane were dissolved 20.2 g (0.1 mol) of diphenylsulfoxide and 26.8 g (0.1 mol) of 2,4-diethylthioxanthene-9-one, and 28.2 g (0.1 mol) of trifluoromethanesulfonic anhydride was added dropwise thereto at −70 to −60° C., followed by gradually warming to room temperature and reacting with stirring for 4 hours. After completion of the reaction, the obtained reaction solution was washed with water (160 ml×4 times) and concentrated under reduced pressure. The obtained crude product was purified by column chromatography to obtain 38.6 g of objective substance as yellow glassy substance (yield: 64%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07318991B2 |
| 出典データセット | uspto-grants-2008_01 |
| ORD ID | ord-59f1c5bee5864c6799ce6232602beaf5 |
| 出典メモ | uspto-grants-2008_01 |