関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Butyloxirane | HCID 15036 | — |
| 反応物 | 1-[2-(3,3,5,5-Tetramethylcyclohexyl)phenyl]piperazine | HCID 11992284 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | HCID 23142297 | HCID 23142297 | 72.6% |
反応手順
A mixture of 1-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine (120 mg, 0.399 mmol) produced in Example (8b), 1,2-epoxyhexane (240 mg, 2.39 mmol) and 2-propanol (0.8 mL) was stirred for 18 hours at an external temperature of 80° C. The reaction mixture was concentrated under reduced pressure to give a residue, which was purified by NH silica gel column chromatography (ethyl acetate/heptane) to give 116 mg of 1-{4-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazin-1-yl}hexan-2-ol as a light yellow solid. This compound (12 mg, 0.030 mmol) was dissolved in diethyl ether and a 4N solution of hydrogen chloride in ethyl acetate (0.0083 mL, 0.033 mmol) was added. The mixed solution was concentrated under reduced pressure and the obtained solid residue was washed with a diethyl ether-heptane mixed solvent and then dried under reduced pressure to give 10 mg of the title compound as a colorless solid.
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-6fa63550bcb241649fefa4e20903c689 |
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| 出典メモ | uspto-grants-2008_09 |
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