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Potassium Carbonate → N-[2-(3,4-Dimethoxyphenyl)ethyl]homopiperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Hexahydro-1,4-diazepine | HCID 68163 | — |
| 反応物 | 4-(2-Chloroethyl)-1,2-dimethoxybenzene | HCID 3015359 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | N-[2-(3,4-Dimethoxyphenyl)ethyl]homopiperazine | HCID 15023608 | 77.1% |
反応手順
32.27 g of homopiperazine, 13.2 g of 2-(3,4-dimethoxyphenyl)ethyl chloride and 71.3 g of potassium carbonate were added to 500 ml of acetonitrile. The obtained mixture was heated under reflux for 20 hours, cooled and filtered. The filtrate was concentrated under a reduced pressure to obtain a residue. This residue was extracted with ether thrice. The extracts were combined, dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated under a reduced pressure. The obtained residue was purified by silica gel column chromatography (solvent: chloroform/methanol/isopropylamine (100:10:1)) to obtain 13.40 g of the title compound as a yellow oil (yield: 77%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05607953 |
| 出典データセット | uspto-grants-1997_03 |
| ORD ID | ord-14df1013ddaf490bb330846c98e166b5 |
| 出典メモ | uspto-grants-1997_03 |