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Triethylamine → 1-(2-Methyl-allyl)-4-(4-nitrophenyl)-piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Chloro-2-methyl-1-propene | HCID 11241 | — |
| 反応物 | 1-(4-Nitrophenyl)piperazine | HCID 80447 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-(2-Methyl-allyl)-4-(4-nitrophenyl)-piperazine | HCID 39975547 | 80.2% |
反応手順
To a solution of 1-(4-nitrophenyl)-piperazine (prepared as described in Reference Example 29; 13 g, 63 mmol) in acetonitrile (150 mL) were added, successively, 3-chloro-2-methyl-propene (6.82 g, 75.4 mmol) and triethylamine (17.6 mL, 126 mmol). The mixture was heated at reflux for 8 hours then the solvent was evaporated under reduced pressure to give a residue which was partitioned between water (150 mL) and ethyl acetate (2×100 mL). The combined organic layers were washed twice with water then dried over sodium sulfate. Filtration and concentration afforded 1-(2-methyl-allyl)-4-(4-nitrophenyl)-piperazine (13.2 g, 79%) as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08524705B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-f81c5b4b7d184514b165c3e29bb5a7ac |
| 出典メモ | uspto-grants-2013_09 |