関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-(2-Bromoethyl)-4-chlorobenzene | HCID 23029 | — |
| 反応物 | 2,2-Diphenyl-5-methylaminopentanamide | HCID 19088475 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2,2-diphenyl-5-[N-(4-chlorophenethyl)-N-methylamino]pentanamide | HCID 19088480 | — |
反応手順
A mixture containing 2,2-diphenyl-5methylaminopentanamide (0.3 g--see Preparation 3), 4-chlorophenethyl bromide (0.234 g--see Preparation 7), anhydrous potassium carbonate (0.4 g) and acetonitrile (10 ml) was heated under reflux for 5 hours. The mixture was concentrated in vacuo and the residue partitioned between dichloromethane (30 ml) and 10% aqueous potassium carbonate (30 ml). The layers were separated and the aqueous layer extracted with dichloromethane (3×20 ml). The combined dichloromethane extracts were dried (MgSO4) and concentrated in vacuo to give a gum which was purified by column chromatography on silica eluting with dichloromethane containing methanol (5% up to 10%). The product-containing fractions were combined and concentrated in vacuo to give the title compound as a gum, yield 0.306 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05302595 |
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| 出典データセット | uspto-grants-1994_04 |
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| ORD ID | ord-99f68429616445159fb740db51b7f098 |
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| 出典メモ | uspto-grants-1994_04 |
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