関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Succinimide | HCID 11439 | — |
| 反応物 | 1-(3-Chloropropyl)-4-(2-methoxyphenyl)piperazine | HCID 622669 | — |
| 触媒 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 2,5-Pyrrolidinedione, 1-[3-[4-(2-methoxyphenyl)-1-piperazinyl]propyl]- | HCID 9949436 | — |
反応手順
1 b Scheme-I: A mixture of 2,5-dioxopyrrolidine (3.68 g, 37.24 mmol), 1-[4-(2-methoxyphenyl)-piperazine-1-yl]-3-chloropropane (10.0 g, 37.24 mmol), potassium carbonate (7.70 g, 55.8 mmol) and tetrabutylammonium bromide (2.38 g, 7.4 mmol) in acetone (100 ml) was refluxed for 12 hours at 80° C. with stirrig. The solvent was evaporated off in vacuo and the residue was taken up in water (80 ml). The aqueous solution was extracted with chloroform (3×50 ml) and the organic layers combined, washed with water (2×50) dried over Na2SO4 and evaporated in vacuo to give the title compound. The product was purified by column chromatography over flash silica gel using chloroforin-methanol (99:1) as eluent; yield 8.00 g (65%) in oil. The hydrochloride salt was prepared by the method described above; mp 199-202° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06812344B1 |
|---|
| 出典データセット | uspto-grants-2004_11 |
|---|
| ORD ID | ord-4ac4da9884994b528a85e33bdb6ac9c1 |
|---|
| 出典メモ | uspto-grants-2004_11 |
|---|