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Acetic Acid → 1-(2-Cyclopropylethyl)-4-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 反応物 | 2-Cyclopropylacetaldehyde | HCID 10307849 | — |
| 反応物 | 1-[2-(3,3,5,5-Tetramethylcyclohexyl)phenyl]piperazine | HCID 11992284 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(2-Cyclopropylethyl)-4-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine | HCID 23141878 | — |
反応手順
To a solution of cyclopropylacetaldehyde in 1,2-dichloroethane (0.29 M, 5 mL) were added 1-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine (25 mg, 0.0832 mmol) produced in Example (8b), sodium triacetoxyborohydride (22.9 mg, 0.108 mmol) and acetic acid (0.009 mL, 0.158 mmol), followed by stirring for 20 minutes at room temperature. Saturated aqueous solution of sodium hydrogencarbonate was added to the reaction mixture and extraction was performed twice with ethyl acetate. The organic layer was concentrated and the resultant residue was purified by NH silica gel column chromatography (ethyl acetate/heptane) to give 20.9 mg of 1-(2-cyclopropylethyl)-4-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine 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-19b23eba74564111ab79266b31c81bff |
| 出典メモ | uspto-grants-2008_09 |