Potassium Carbonate → HCID 4715098、化合物

HRID 1748492ノート

反応式

HRID 1748492 の反応式
FC(F)(F)S(O)(=O)=O.[F:9][C:10]1[CH:15]=[CH:14][C:13]([N:16]2[CH:20]=[CH:19][CH:18]=[C:17]2C=O)=[CH:12][CH:11]=1.[C:23](=O)([O-])[O-:24].[K+].[K+]>ClCCl>[F:9][C:10]1[CH:11]=[CH:12][C:13]([N:16]2[CH:17]=[CH:18][C:19]([CH:23]=[O:24])=[CH:20]2)=[CH:14][CH:15]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 62406Trifluoromethanesulfonic acidHCID 31618451-(4-fluorophenyl)-1H-pyrrole-2-carbaldehyde

生成物 1

HCID 4715098HCID 4715098、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Trifluoromethanesulfonic acid (100 g) was added dropwise at room temperature into a dichloromethane solution (680 ml) containing 1-(4-fluorophenyl)-2-formylpyrrole (50.4 g), and stirred at reflux temperature for 13 hours. The reaction solution was poured into ice water, made alkaline with the addition of potassium carbonate and extracted with chloroform. The organic layer was dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified with silica gel column chromatography (n-hexane/ethyl acetate) to give 1-(4-fluorophenyl)-3-formylpyrrole (34.5 g).

後処理

  1. temperatureat reflux temperature for 13 hours
  2. extractionextracted with chloroform
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified with silica gel column chromatography (n-hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-277d9dd4c88240bcbac2045e55be618a
出典データセット
uspto-grants-2015_10
特許番号
US09150555B2

反応ノート

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