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Triethylamine → 1-(2-Chlorophenyl)-4-{2-[bis(4-hydroxyphenyl)methyl]benzyl}piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-(2-Chlorophenyl)piperazine | HCID 415628 | — |
| 反応物 | 2-[Bis(4-hydroxyphenyl)methyl]benzylbromide | HCID 19938176 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(2-Chlorophenyl)-4-{2-[bis(4-hydroxyphenyl)methyl]benzyl}piperazine | HCID 19938118 | 14.6% |
反応手順
In 50 ml of tetrahydrofuran were dissolved 1.5 g of 1-(2-chlorophenyl)piperazine and 5 ml of triethylamine, and 3.4 g of 2-[bis(4-hydroxyphenyl)methyl]benzylbromide was added thereto. The mixture was heated under reflux for 3.5 hours, and then insoluble substances were filtered off. The filtrate was concentrated, and the residue was subjected to extraction with the addition of water and ethyl acetate. The organic layer was separated, and the aqueous layer was then extracted with ethyl acetate. The organic layers were combined and then dried over anhydrous magnesium sulfate. The solvent was evaporated off under reduced pressure, and the residue was purified by silica gel chromatography to afford 0.54 g of the desired compound (Compound 89).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05413997 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-0208c64273a84e8e8c4fda96508a2f39 |
| 出典メモ | uspto-grants-1995_05 |