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Triethylamine → ethyl 6-[N'-(3-chlorophenyl)-N-piperazinyl]hexanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-(3-Chlorophenyl)piperazine monohydrochloride | HCID 25681 | — |
| 反応物 | Ethyl 6-bromohexanoate | HCID 117544 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | ethyl 6-[N'-(3-chlorophenyl)-N-piperazinyl]hexanoate | HCID 67128506 | 59.6% |
反応手順
To a solution of 1-(3-chlorophenyl)piperazine hydrochloride (12 g, 0.051 mol) in anhydrous toluene (250 ml) was added triethylamine (TEA) (15.6 ml, 0.112 mol) and ethyl 6-bromohexanoate (13.6 g, 0.061 mol) and the mixture heated at reflux for 4 hours. The mixture was then cooled to room temperature, washed with water (2×100 ml), brine (100 ml), dried over Na2SO4, filtered and concentrated to dryness. The residue obtained was purified by flash chromatography on silica gel using ethyl acetate/hexane (1/1) to give ethyl 6-[N′-(3-chlorophenyl)-N-piperazinyl]hexanoate (10.3 g) as a clear oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08476029B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-0dcef08f389c4c03a153929326d5e18b |
| 出典メモ | uspto-grants-2013_07 |