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Chlorodifluoromethane → 4-Chloro-4'-difluoromethylthiomethyl-benzophenone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chlorodifluoromethane | HCID 6372 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | 4-Chloro-4'-mercaptomethylbenzophenone | HCID 19689380 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Chloro-4'-difluoromethylthiomethyl-benzophenone | HCID 19689369 | 36% |
反応手順
4-chloro-4'-mercaptomethylbenzophenone (14.7 g) and potassium hydroxide (15 g) was added to a solvent comprising dioxane (100 ml) and water (100 ml). Difluoromethyl chloride was blown into this solution at 60° C. until the starting material 4-chloro-4'-mercaptomethylbenzophenone disappeared. The reaction product was cooled to room temperature and then subjected to filtration. The organic layer as the filtrate was dried over anhydrous magnesium sulfate add concentrated. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=5:1) to obtain the desired product (6.4 g, melting point: 34° to 35° C., yield: 36%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05728699 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-54662bdd64d74fb6bcb38cb65a7a5fc0 |
| 出典メモ | uspto-grants-1998_03 |