Diethyl Ether → 1-[[[4-(Phenylmethyl)-1-piperazinyl]carbonyl]amino]cyclohexanecarboxylic acid

HRID 1851807노트

반응식

HRID 1851807 반응식
[OH-].[Na+].C([O:5][C:6]([C:8]1([NH:14][C:15]([N:17]2[CH2:22][CH2:21][N:20]([CH2:23][C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH2:19][CH2:18]2)=[O:16])[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1)=[O:7])C.CCOCC>C(O)C>[C:24]1([CH2:23][N:20]2[CH2:19][CH2:18][N:17]([C:15]([NH:14][C:8]3([C:6]([OH:7])=[O:5])[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]3)=[O:16])[CH2:22][CH2:21]2)[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 14798Sodium HydroxideHCID 57672921HCID 57672921, 화합물

생성물 1

HCID 576729481-[[[4-(Phenylmethyl)-1-piperazinyl]carbonyl]amino]cyclohexanecarboxylic acid수율 42%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

600 ml of 1N aqueous sodium hydroxide solution was added to a solution of 7.62 g (20 mmol) of 1-[[(4-phenylmethyl-1-piperazinyl)carbonyl]amino]cyclohexanecarboxylic acid ethyl ester in 300 ml of ethanol, and the mixture was heated under reflux for 2 hours. After ether was added to the reaction solution and the mixture was washed, the aqueous layer was neutralized by concentrated hydrochloric acid and extracted with ethyl acetate. After the obtained organic layer was washed with saturated brine, the layer was dried with anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain 2.90 g (42%) of the title compound.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2 hours
  3. washthe mixture was washed
  4. extractionextracted with ethyl acetate
  5. washAfter the obtained organic layer was washed with saturated brine
  6. dry with materialthe layer was dried with anhydrous sodium sulfate
  7. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-9d2371707e704e28b0258a339f02222b
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957205B2

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