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Benzyl Bromide → 5-(3,4-Dimethoxyphenyl)-2-benzylpyrazolin-3-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzyl Bromide | HCID 7498 | — |
| 反応物 | 2,4,6-Trimethylpyridine | HCID 7953 | — |
| 反応物 | 5-(3,4-Dimethoxyphenyl)-pyrazolin-3-one | HCID 22046088 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-(3,4-Dimethoxyphenyl)-2-benzylpyrazolin-3-one | HCID 22902338 | — |
反応手順
5 g of 5-(3,4-dimethoxyphenyl)-pyrazolin-3-one, prepared according to Example 1C, were suspended in 100 ml of toluene. First 3 ml of collidine and subsequently 3.6 ml of benzyl bromide were added dropwise to the suspension. After heating for 6 hours under reflux, the reaction mixture was cooled, and the precipitated crystals were filtered out and washed with isopropanol. The crystals obtained were dissolved in dichloromethane and washed with 2M citric acid. The organic phase was dried with magnesium sulfate and concentrated. For purification the residue was recrystallized from isopropanol. 4 g of 5-(3,4-dimethoxyphenyl)-2-benzyl-pyrazolin-3-one were obtained having a melting point of 165° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05679699 |
| 出典データセット | uspto-grants-1997_10 |
| ORD ID | ord-b9eec5786b4c43f888099167371f7d17 |
| 出典メモ | uspto-grants-1997_10 |