関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-(2-Bromoethyl)-4-methoxybenzene | HCID 84427 | — |
| 反応物 | (Benzo[b]thiophene-3-yl)(4-piperidinyl)methanone | HCID 15337457 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | [Benzo[b]thiophene-3-yl][1-[2-(4-methoxyphenyl)ethyl]-4-piperidinyl]methanone | HCID 9799982 | — |
反応手順
Mix (benzo[b]thiophene-3-yl)(4-piperidinyl)methanone.CF3CO2H (2.0 g, 5.56 mmol), 2-(4-methoxyphenyl)ethyl bromide (1.27 g, 5.93 mmol), potassium carbonate (1.95 g, 1.41 mmol) and anhydrous dimethylformamide (20 mL). Warm to approximately 90° C. and stir overnight. Allow to cool to room temperature and partition between a 2:1 mixture of ethyl acetate:toluene and water. Separate the aqueous phase and wash the organic phase with water and saturated sodium chloride. Dry (Na2SO4) and evaporate the solvent in vacuo. Purify by chromatography (40% ethyl acetate/hexane) and recrystallize (cyclohexane) to give the title compound as pale yellow plates; mp 114°-116° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05541200 |
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| 出典データセット | uspto-grants-1996_07 |
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| ORD ID | ord-d32c1cb8f02c490683939e8dda47f6dc |
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| 出典メモ | uspto-grants-1996_07 |
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