関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | p-Fluorophenyl 4-piperidyl ketone hydrochloride | HCID 3084438 | — |
| 反応物 | 1-(4-chlorobutyl)-1,3-dihydro-2H-benzimidazol-2-one | HCID 13360889 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Methyl Isobutyl Ketone | HCID 7909 | — |
| 生成物 | 1-{4-[4-(4-fluorobenzoyl)-1-piperidinyl]butyl}-1,3-dihydro-2H-benzimidazol-2-one | HCID 54155158 | 30% |
反応手順
A mixture of 4 parts of 1-(4-chlorobutyl)-1,3-dihydro-2H-benzimidazol-2-one, 4 parts of (4-fluorophenyl) (4-piperidinyl) methanone hydrochloride, 10 parts of sodium carbonate, 0.2 parts of potassium iodide and 80 parts of 4-methyl-2-pentanone is stirred and refluxed overnight. After cooling, water is added and the layers are separated. The organic phase is dried, filtered and evaporated. The solid residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and 10% of methanol as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from 4-methyl-2-pentanone, yielding 2 parts (30%) of 1-{4-[4-(4-fluorobenzoyl)-1-piperidinyl]butyl} -1,3-dihydro-2H-benzimidazol-2-one; mp. 176.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04035369 |
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| 出典データセット | uspto-grants-1977_07 |
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| ORD ID | ord-fc9d249e84de44eebf843f8c59c1d2ba |
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| 出典メモ | uspto-grants-1977_07 |
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