Ammonium Hydroxide → 3-Cyclohexylpyrrolidin-2-one

HRID 1670812ノート

反応式

HRID 1670812 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 576579993-Cyclohexylpyrrolidin-2-one収率 94%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c2deaf126d1e4c1a91c00912e7ccb0ee
出典データセット
uspto-grants-2011_08
特許番号
US07994176B2

反応ノート

読み込み中…