関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,3-Cyclopentanedicarboxylic acid | HCID 107216 | — |
| 反応物 | 1-(4-Aminobutyl)-4-benzylpiperazine hydrochloride | HCID 20137499 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | HCID 178478895 | HCID 178478895 | — |
反応手順
1,3-Cyclopentane dicarboxylic acid (8.0 g., 51 mmole) was converted to the anhydride by refluxing for 3 hours in 100 ml. of acetic anhydride. The excess solvent was removed under vacuum and the residue was stored in vacuum for 18 hours. The crude anhydride thus obtained was combined with 14 g. (50 mmole) of 1-(4-aminobutyl)-4-benzylpiperazine hydrochloride and 5.0 g. (50 mmole) of triethylamine in 500 ml. of xylene. The mixture was refluxed for 48 hours with water separation via a Dean-Stark trap. The product was concentrated under vacuum and chromatographed on 200 g. of silica gel with 2% ethanol/chloroform. The product was crystallized from ethanol by addition of 4N HCl/isopropyl alcohol to obtain cyclopentane-1,3-dicarboxylic-N-[4-(4-benzyl-1-piperazinyl)butyl]imide dihydrochloride; m.p. 273°-275° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04748240 |
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| 出典データセット | uspto-grants-1988_05 |
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| ORD ID | ord-08521a6b0d0b4fd3934f670411b3b9a9 |
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| 出典メモ | uspto-grants-1988_05 |
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