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Hydrochloric Acid → 1-{3-[4-(4-Chlorobenzyl)piperazin-1-yl]propyl}-3-(4-carbamylphenyl)urea dihydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 1-{3-[4-(4-Chlorobenzyl)piperazin-1-yl]propyl}-3-(4-cyanophenyl)urea dihydrochloride monohydrate | HCID 20205727 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 1-{3-[4-(4-Chlorobenzyl)piperazin-1-yl]propyl}-3-(4-carbamylphenyl)urea dihydrochloride | HCID 13606710 | 70.8% |
反応手順
A solution of 1-{3-[4-(4-chlorobenzyl)piperazin-1-yl]-propyl}-3-(4-cyanophenyl)urea dihydrochloride monohydrate (10.0 g; 19.9 mmole), glacial acetic acid (120 ml), and concentrated hydrochloric acid (80 ml) was heated at 80° C. for 30 minutes. The mixture was then poured over ice, and basified with aqueous potassium hydroxide. The product was extracted with methylene chloride, dried (sodium sulfate), and the salt precipitated out ethereal hydrochloric acid. Several recrystallizations from ethanol provided the title compound (3.54 g; 38% yield) as colorless crystals, m.p. 224°-226° 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-51c67029f83146d29e0f26850ea302ec |
| 出典メモ | uspto-grants-1987_04 |