関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Piperazine | HCID 4837 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 1,1'-(Chloromethylene)bis(4-fluorobenzene) | HCID 2723773 | — |
| 反応物 | Dichloromethane methanol | HCID 21226129 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 1-(Bis(4-fluorophenyl)methyl)piperazine | HCID 152932 | 78.3% |
反応手順
To 14.32 g (60 mmol) of said 4,4'-difluorobenzhydryl chloride were added 10.46 g (90 mmol) of anhydrous sodium carbonate, 25.84 g (300 mmol) of piperazine and 52 ml of dry chloroform, and the mixture was heated under reflux. To the reaction mixture was added dropwise over 45 minutes 14.32 g (60 mmol) of 4,4'-difluorobenzhydryl chloride in 13 ml of dry chloroform. The mixture was heated under reflux for 18 hours and filtered. The filtrate was washed successively with water and a saturated aqueous sodium chloride solution, and the organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. There was obtained a residue, which was subjected to column chromatography on silica gel to give 13.49 g (47 mmol) of 4,4'-difluorobenzhydryl piperazine from eluates of dichloromethane-methanol (10:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04792553 |
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| 出典データセット | uspto-grants-1988_12 |
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| ORD ID | ord-3832c891265b4c79b4ff43f0080d0074 |
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| 出典メモ | uspto-grants-1988_12 |
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