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Dimethylformamide → HCID 58629126、化合物

HRID 1678059
ノート
印刷プレビュー

反応式

HRID 1678059 の反応式
[CH3:1][C:2](C)([O-])[CH3:3].[K+].[NH:7]1[CH:11]=[CH:10][C:9]([C:12](=[O:14])[CH3:13])=[CH:8]1.CN(C=O)C.IC(C)C>CCOCC.O>[CH:2]([N:7]1[CH:11]=[CH:10][C:9]([C:12](=[O:14])[CH3:13])=[CH:8]1)([CH3:3])[CH3:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 6362Isopropyl iodideHCID 27377933-AcetylpyrroleHCID 23665647Potassium tert-butoxide

生成物 1

HCID 58629126HCID 58629126、化合物収率 56.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 3283
Diethyl Ether
溶媒

実験手順

Potassium t-butoxide (6.7 g, 60 mmol) was added to a stirred 0° C. solution of 1-(1H-pyrrol-3-yl)ethanone (5.0 g, 46 mmol) of DMF (150 mL). After stirring for 30 minutes, 2-iodopropane (10.1 g, 60 mmol) was added and the mixture was stirred overnight at approximately 25° C. The mixture was diluted with Et2O and H2O. The portions were separated, and the aqueous portion was extracted two more times. The organic portions were combined and washed with brine and then dried with Na2SO4. The mixture was filtered and the solvent removed in vacuo. The crude product was purified by flash chromatography (30 percent ether/pentane over silica gel), affording 3.9 g of yellow oil.

後処理

  1. stirringthe mixture was stirred overnight at approximately 25° C
  2. customThe portions were separated
  3. extractionthe aqueous portion was extracted two more times
  4. washwashed with brine
  5. dry with materialdried with Na2SO4
  6. filtrationThe mixture was filtered
  7. customthe solvent removed in vacuo
  8. customThe crude product was purified by flash chromatography (30 percent ether/pentane over silica gel)

出典と根拠

ORDレコード
ord-43705e5815e04005ab7b400c2e27adf4
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08008487B2

反応ノート

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