関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-(4-Pyridyl)piperazine | HCID 70517 | — |
| 反応物 | Ethyl 2-[4-(2-bromoacetyl)phenoxy]acetate | HCID 18408936 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Ethyl 4-[2-[4-(4-pyridyl)piperazin-1-yl]acetyl]phenoxyacetate | HCID 18918266 | — |
反応手順
Ethyl 4-bromoacetylphenoxyacetate (6.0 g) was added to a stirred, cooled (4° C.) solution of 1-(4-pyridyl)piperazine (6.5 g) in acetonitrile (225 ml). Stirring was continued for 1 hour at 4° C., then overnight at ambient temperature when the precipitated solid was removed by filtration. The filtrate was evaporated in vacuo and the solid residue triturated with water, filtered, then washed with water and dried. Recrystallization from a small volume of ethanol gave the title compound, 1.71 g, as a cream coloured solid: m.p. 113°-114° C.; NMR (d6DMSO) δ8.15(2H,d), 7.98(2H,d), 7.02(2H,d), 6.80(2H,d), 4.89(2H,d), 4.17(2H,q), 3.84(2H,s), 3.32(4H,t), 2.62(4H,t) 1.22(3H,t); m/e 384 (M+H)+ ; calculated for C21H25N3O4 : C, 65.8; H, 6.6; N, 11.0. found: C, 65.5; H, 6.6; N, 10.8%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05750754 |
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| 出典データセット | uspto-grants-1998_05 |
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| ORD ID | ord-ca3c42b492ea439fa1bd5336aa38c091 |
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| 出典メモ | uspto-grants-1998_05 |
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