関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Boron trifluoride etherate | HCID 8000 | — |
| 反応物 | Isobutylene oxide | HCID 11208 | — |
| 反応物 | 1-Cyclohexylethanol | HCID 137829 | — |
| 溶媒 | Cyclohexane | HCID 8078 | — |
| 生成物 | 2-(1-Cyclohexylethoxy)-2-methyl-1-propanol | HCID 22053299 | 66.1% |
反応手順
BF3—OEt2 (2.0 ml) is added dropwise to a solution of 1-cyclohexylethanol (16.6 g, 127.0 mmol) and isobutylene oxide (2.9 g, 40.0 mmol) in cyclohexane (20 ml) that has been cooled to 0° C. The reaction mixture is now stirred at 0° C. for a further 30 minutes, and further, BF3—OEt2 (2.0 ml) is then added. After a further 3 hours at 0° C., the cooling is removed and the reaction solution is washed once with 1 M NaOH (15 ml). The organic phase is dried over Na2SO4, filtered off and freed from solvent in a rotary evaporator. The 1-cyclohexylethanol that has not completely reacted is removed from the crude product; thus, obtained by means of bulb tube distillation (BTD) and 5.3 g crude 2-(1-cyclohexylethoxy)-2-methyl-1-propanol is obtained which has a GC content of 75% and can be used in the next reaction without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07064102B2 |
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| 出典データセット | uspto-grants-2006_06 |
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| ORD ID | ord-27d36f7e05ac4c0799ed0dd01f66ed6f |
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| 出典メモ | uspto-grants-2006_06 |
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