Cyclohexylpyrrolidinium hydrochloride salt → 1-Cyclohexylpyrrolidine

HRID 514645

反応式

HRID 514645 の反応式
Cl.[CH:2]1([NH+:8]2[CH2:12][CH2:11][CH2:10][CH2:9]2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1>O>[CH:2]1([N:8]2[CH2:12][CH2:11][CH2:10][CH2:9]2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1

参加物

3

反応物 1

HCID 131733292Cyclohexylpyrrolidinium hydrochloride salt

生成物 1

HCID 1390641-Cyclohexylpyrrolidine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  1. customis separated
  2. extractionThe free cyclohexylpyrrolidine is extracted with ethyl acetate
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated on a rotary evaporator at reduced pressure

出典と根拠

ORDレコード
ord-8d54c468fe694162aa87f9dd325baa01
出典データセット
uspto-grants-2015_08
特許番号
US09108856B2

関連ノート

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