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Acetic Acid → 1-(2-Bromophenyl)-4-cyclopropylmethylpiperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Cyclopropanecarboxaldehyde | HCID 123114 | — |
| 反応物 | 1-(2-Bromophenyl)piperazine | HCID 2757153 | — |
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(2-Bromophenyl)-4-cyclopropylmethylpiperazine | HCID 23142839 | 103.1% |
反応手順
To a solution of 1-(2-bromophenyl)piperazine (3.0 g, 12.4 mmol) in tetrahydrofuran (30 mL) were added acetic acid (0.71 mL, 12.4 mmol), cyclopropanecarbaldehyde (1.39 mL, 18.66 mmol) and sodium triacetoxyborohydride (4.22 g, 19.9 mmol), followed by stirring for 88 hours at room temperature. Aqueous solution of potassium carbonate was added to the reaction mixture, extraction was performed with ethyl acetate, and the organic layer was concentrated. The resultant residue was purified by NH silica gel column chromatography (ethyl acetate/heptane) to give 3.773 g of the title compound as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07425554B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-c185f7e84db146ab9a55b333dfe511a7 |
| 出典メモ | uspto-grants-2008_09 |