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Triethylamine → 1-{3-[4-(4-Chlorobenzyl)piperazin-1-yl]propyl}-3-allylurea dihydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Allyl isocyanate | HCID 15123 | — |
| 反応物 | 1-(3-Aminopropyl)-4-(4-chlorobenzyl)piperazine trihydrochloride | HCID 20205739 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-{3-[4-(4-Chlorobenzyl)piperazin-1-yl]propyl}-3-allylurea dihydrochloride | HCID 13606696 | 49.6% |
反応手順
A solution of triethylamine (2.0 g; 20 mmole) in methylene chloride was added dropwise to a mixture of 1-(3-amino-propyl)-4-(4-chlorobenzyl)piperazine trihydrochloride (7.54 g; 20 mmole) and allyl isocyanate (1.66 g; 20 mmole) in methylene chloride. After the addition was completed the mixture was washed with water and the solvent removed. The resulting orange oil was purified on a silica gel column (methylene chloride/methanol; 9:1), precipitated with ethereal hydrochloric acid, and recrystallized from ethanol/water to provide the title compound (2.1 g; 25% yield) as colorless crystals, m.p. 232°-234° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04661481 |
| 出典データセット | uspto-grants-1987_04 |
| ORD ID | ord-30b36e18d315416f89acb89c29e0e57d |
| 出典メモ | uspto-grants-1987_04 |