化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → N-[2-(Phenylsulfonyl)ethyl]-1-homopiperidineethanamine maleate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | ((2-Chloroethyl)sulphonyl)benzene | HCID 13646 | — |
| 反応物 | Hexahydro-1H-azepine-1-ethanamine | HCID 40002 | — |
| 反応物 | Maleic Acid | HCID 444266 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | N-[2-(Phenylsulfonyl)ethyl]-1-homopiperidineethanamine maleate | HCID 70360557 | 60.7% |
反応手順
A mixture of 20.06 g (0.098 mole) of [(2-chloroethyl)sulfonyl]benzene 15.44 g (0.109 mole) of N-(2-aminoethyl)homopiperidine, and 15.0 g (0.149 mole) of triethylamine in 800 ml of acetonitrile was stirred at room temperature for 18 hr. The solvent was removed in vacuo, and the residue was partitioned between methylene chloride and water. The methylene chloride solution was dried over magnesuim sulfate, and the solvent waas removed in vacuo to give an oil. This was dissolved in methanol, and the solution was treated with a solution of 2 equivalents of maleic acid (25.52 g, 0.22 mole) in methanol. A white solid precipitated at room temperature to give 32.3 g (60.7%) of title compound as a white solid; mp 144°-146° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04895840 |
| 出典データセット | uspto-grants-1990_01 |
| ORD ID | ord-79450b90b97243f09b921d594904fb8c |
| 出典メモ | uspto-grants-1990_01 |