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6-Hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylcarbonyl}-1,4-benzodioxin → 6-Hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylmethyl}-1,4-benzodioxin
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 6-Hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylcarbonyl}-1,4-benzodioxin | HCID 9804471 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 6-Hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylmethyl}-1,4-benzodioxin | HCID 10433893 | 85% |
反応手順
Under a nitrogen atmosphere, heat at reflux for 3 hours, in the presence of 5 mmol of lithium aluminium hydride, a solution of 2 mmol of 6-hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylcarbonyl}-1,4-benzodioxin in 35 cm3 of diethyl ether. After cooling, hydrolysis, removal of the insoluble mineral compounds by filtration and drying over magnesium sulfate, the compound obtained is purified by chromatography on a column of silica (eluant: petroleum ether/ethyl acetate, 40:60). 6-Hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylmethyl}-1,4-benzodioxin is thereby obtained in a yield of 85%. Melting point: 190° C. ##STR79##
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05439909 |
| 出典データセット | uspto-grants-1995_08 |
| ORD ID | ord-7ed4eb78a0524eab842045f9adfce8f8 |
| 出典メモ | uspto-grants-1995_08 |