Ammonium Hydroxide → 3-Cyclohexylpyrrolidin-2-one

HRID 1670812노트

반응식

HRID 1670812 반응식
[CH:1]1([CH:7]2[CH2:11][CH2:10][O:9][C:8]2=O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[OH-].[NH4+:14]>C(O)C>[CH:1]1([CH:7]2[CH2:11][CH2:10][NH:14][C:8]2=[O:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

4

반응물 2

HCID 14923Ammonium HydroxideHCID 220132343-Cyclohexyl-dihydro-furan-2-one

생성물 1

HCID 576579993-Cyclohexylpyrrolidin-2-one수율 94%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Heat a mixture of 3-cyclohexyl-dihydro-furan-2-one (32.2 g), ammonium hydroxide (700 mL) and ethanol (700 mL) at 230° C. in a sealed steel bottle for 18 hours. Cool the reaction and remove the solvent in vacuo. Partition the residue with ethyl acetate (500 mL) and HCl (1N, 300 mL). Dry the organic over sodium sulfate. After filtration and concentration, recrystallize with 1:3 ethyl acetate:hexane to afford 30 grams (94%) of the title compound.

후처리

  1. temperatureHeat
  2. temperatureCool
  3. customthe reaction
  4. customremove the solvent in vacuo
  5. customPartition the residue with ethyl acetate (500 mL) and HCl (1N, 300 mL)
  6. dry with materialDry the organic over sodium sulfate
  7. filtrationAfter filtration and concentration
  8. customrecrystallize with 1:3 ethyl acetate

출처 및 근거

ORD 기록
ord-c2deaf126d1e4c1a91c00912e7ccb0ee
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07994176B2

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