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1-Bromo-3-chloropropane → 1-(4-Chlorobenzyl)-4-(3-chloropropyl)homopiperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Bromo-3-chloropropane | HCID 8006 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 1-[(4-Chlorophenyl)methyl]-1,4-diazepane | HCID 15634377 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 1-(4-Chlorobenzyl)-4-(3-chloropropyl)homopiperazine | HCID 20153188 | 42% |
反応手順
15.7 g of 1-bromo-3-chloropropane were added to a cooled solution of 15.0 g of 1-(4-chlorobenzyl)homopiperazine and 12.0 g of potassium hydroxide in 50 ml of dimethyl sulfoxide. The mixture was stirred at 5°-10° C. for one hour, and then an additional 30 minutes at room temperature. After the addition of ice water, the product was extracted with ether, and the extract was dried (magnesium sulfate) and concentrated in vacuo. Final purification was effected on a silica gel column (methylene chloride:methanol, 9:1), and the solvent was removed in vacuo to give 8.4 g (42% of theory) of 1-(4-chlorobenzyl)-4-(3-chloropropyl)homopiperazine as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04618677 |
| 出典データセット | uspto-grants-1986_10 |
| ORD ID | ord-5ccc732570e64ea09e94a3855cb22b8d |
| 出典メモ | uspto-grants-1986_10 |