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Thionyl Chloride → 1,1'-(Chloromethylene)bis(4-fluorobenzene)
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 4,4'-Difluorobenzhydryl alcohol | HCID 123049 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1,1'-(Chloromethylene)bis(4-fluorobenzene) | HCID 2723773 | 90.3% |
反応手順
To 5.00 g (22.7 mmol) of 4,4'-difluorobenzhydrol was added 16.5 ml (227 mmol) of thionyl chloride in the atmosphere of argon, and the mixture was stirred at room temperature for 30 minutes. To the resulting mixture was added water followed by extraction with benzene. The organic layer was successively washed with saturated sodium hydrogen carbonate solution and water, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue thus obtained was subjected to column chromatography on silica gel. There was yielded 4.90 g (20.5 mmol) of 4,4'-difluorobenzhydryl chloride from the fraction eluted with benzene.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04792553 |
| 出典データセット | uspto-grants-1988_12 |
| ORD ID | ord-3105e40af57f46429c343abecd5a1306 |
| 出典メモ | uspto-grants-1988_12 |