関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Fluoro-6-methoxyaniline | HCID 459253 | — |
| 反応物 | Ethanamine, 2-bromo-N-(2-bromoethyl)-, hydrobromide (1:1) | HCID 12692731 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(2-Fluoro-6-methoxyphenyl)piperazine | HCID 15676121 | 77% |
反応手順
2-Fluoro-6-methoxyaniline (7.80 g) and 17.23 g of di-(2-bromoethyl)amine hydrobromide were dissolved in 5 ml of water and, by heating at about 110° C. on a bath, 10 ml of 30% potassium hydroxide solution was added thereto (each about 3.5 ml once an hour). Heating was further continued (7 hours in total). After cooled, the reaction solution was made alkaline with aqueous solution of sodium hydroxide to salt out and extracted with chloroform twice. The extract was washed with saturated sodium chloride solution, dried over sodium sulfate, the solvent was evaporated therefrom, and the residue was purified by a column chromatography to give 8.95 g of oily 1-(2-fluoro-6-methoxyphenyl)piperazine in 34.93 g yield or 94%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05086049 |
|---|
| 出典データセット | uspto-grants-1992_02 |
|---|
| ORD ID | ord-4221356c531047a2a9f8568c1e0db29d |
|---|
| 出典メモ | uspto-grants-1992_02 |
|---|