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Potassium Carbonate → diethyl 5-benzoyl-2,3-dihydro-1H-pyrrolizine-1,1-dicarboxylate

HRID 1090818
ノート
印刷プレビュー

反応式

HRID 1090818 の反応式
[C:1]([C:9]1[NH:13][C:12]([C:14]([C:25]([O:27][CH2:28][CH3:29])=[O:26])([C:20](OCC)=O)[C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:11][CH:10]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:30](=O)([O-])[O-].[K+].[K+]>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.ClCCCl>[C:1]([C:9]1[N:13]2[C:12](=[CH:11][CH:10]=1)[C:14]([C:15]([O:17][CH2:18][CH3:19])=[O:16])([C:25]([O:27][CH2:28][CH3:29])=[O:26])[CH2:20][CH2:30]2)(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 11430Potassium CarbonateHCID 11069430Triethyl (5-benzoyl-1H-pyrrol-2-yl)methanetricarboxylate

生成物 1

HCID 9928574diethyl 5-benzoyl-2,3-dihydro-1H-pyrrolizine-1,1-dicarboxylate収率 80%

試薬・触媒・溶媒 2

HCID 74236Tetrabutylammonium Bromide触媒HCID 111,2-Dichloroethane溶媒

実験手順

A mixture of triethyl (5-benzoylpyrrol-2-yl)-methanetricarboxylate (2.00 g, 5 mmol), tetra-butylammonium bromide (1.61 g, 5 mmol) and potassium carbonate (19.0 g, 250 mmol) in 1,2-dichloroethane (100 mL) was refluxed for 2 days. The mixture was cooled to room temperature and filtered. The filter cake was washed with methylene chloride. The filtrate and methylene chloride wash solution were combined and concentrated under reduced pressure. The residue was dissolved in diethyl ether, washed with water, dried, and concentrated. The crude product was purified by flash chromatography on flash silica eluting with hexane/ethyl acetate (90:10) to provide 1.42 g (80%) of diethyl 5-benzoyl-2,3-dihydro-1H-pyrrolizine-1,1-dicarboxylate. The IR and NMR spectral properties were identical to those of the authentic sample.

後処理

  1. temperaturewas refluxed for 2 days
  2. filtrationfiltered
  3. washThe filter cake was washed with methylene chloride
  4. washThe filtrate and methylene chloride wash solution
  5. concentrationconcentrated under reduced pressure
  6. dissolutionThe residue was dissolved in diethyl ether
  7. washwashed with water
  8. customdried
  9. concentrationconcentrated
  10. customThe crude product was purified by flash chromatography on flash silica eluting with hexane/ethyl acetate (90:10)

出典と根拠

ORDレコード
ord-814ff16ec40e4c6c87c3ce3c4e120972
出典データセット
uspto-grants-1992_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05082950

反応ノート

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