Cyclohexylpyrrolidinium hydrochloride salt → 1-Cyclohexylpyrrolidine

HRID 514645

반응식

HRID 514645 반응식
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

참가 물질

3

반응물 1

HCID 131733292Cyclohexylpyrrolidinium hydrochloride salt

생성물 1

HCID 1390641-Cyclohexylpyrrolidine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8d54c468fe694162aa87f9dd325baa01
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09108856B2

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