関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cyclohexylpyrrolidinium hydrochloride salt | HCID 131733292 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Cyclohexylpyrrolidine | HCID 139064 | — |
反応手順
In some instances when some unreacted cyclohexanone is still in the reaction mixture, the product after hydrogenation was purified by adding 3M HCl solution to the mixture (after filtering out the palladium/carbon catalyst) and left to stir for 15-20 minutes. The resulting mixture was then extracted with diethyl ether to remove the cyclohexanone from the mixture and leaving behind the cyclohexylpyrrolidinium hydrochloride salt. The water layer containing cyclohexylpyrrolidinium hydrochloride salt is separated and then neutralized with NaOH solution to a pH of 9-10. The free cyclohexylpyrrolidine is extracted with ethyl acetate, dried over MgSO4 and concentrated on a rotary evaporator at reduced pressure to give the desired product free from any impurities.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09108856B2 |
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| 出典データセット | uspto-grants-2015_08 |
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| ORD ID | ord-8d54c468fe694162aa87f9dd325baa01 |
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| 出典メモ | uspto-grants-2015_08 |
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