関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Allyl bromide | HCID 7841 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 1-[2-(3,3,5,5-Tetramethylcyclohexyl)phenyl]piperazine | HCID 11992284 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Dichloromethane ethylacetate | HCID 21226138 | — |
| 生成物 | 1-Allyl-4-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine | HCID 23141803 | — |
反応手順
A mixture of 1-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine (30 mg, 0.1 mmol) produced in Example (8b), allyl bromide (14.8 mg, 0.12 mmol), potassium carbonate (20.8 mg, 0.15 mmol) and dimethylformamide (1 mL) was stirred for 4 hours and 20 minutes at an external temperature of 80° C. Saturated aqueous solution of sodium hydrogencarbonate was added to the reaction mixture and extraction was performed with ethyl acetate-dichloromethane. The separated organic layer was washed with water, and then the solvent was distilled off by nitrogen stream. The resultant residue was purified by NH silica gel column chromatography (ethyl acetate/heptane) to give 1-allyl-4-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07425554B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-00d379097aaf48f39b85028bf376efd8 |
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| 出典メモ | uspto-grants-2008_09 |
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