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Potassium Carbonate → HCID 15005406、化合物

HRID 1672538
ノート
印刷プレビュー

反応式

HRID 1672538 の反応式
[CH:1]([C:3]1[CH:10]=[CH:9][C:6]([C:7]#[N:8])=[CH:5][CH:4]=1)=[O:2].[N+:11]([CH:13](S(C1C=CC(C)=CC=1)(=O)=O)[CH3:14])#[C-:12].C(=O)([O-])[O-].[K+].[K+]>CO>[CH3:14][C:13]1[N:11]=[CH:12][O:2][C:1]=1[C:3]1[CH:10]=[CH:9][C:6]([C:7]#[N:8])=[CH:5][CH:4]=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 3

HCID 11430Potassium CarbonateHCID 660424-CyanobenzaldehydeHCID 110528851-(1-Isocyanoethanesulfonyl)-4-methylbenzene

生成物 1

HCID 15005406HCID 15005406、化合物収率 75%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

4-Formylbenzonitrile (1.61 g, 12.3 mmol), 1-(1-isocyanoethylsulfonyl)-4-methylbenzene (2.58 g, 12.3 mmol), and potassium carbonate (3.39 g, 24.5 mmol) in methanol (60 mL) was heated to reflux overnight. The reaction mixture was cooled and the volatiles evaporated. The residue was partitioned between water and ethyl acetate. The organic phase was washed with water and brine, dried over Na2SO4, filtered, and evaporated. The solid was chromatographed on silica gel, eluting with 10% to 50% ethyl acetate:hexanes to afford 1.70 g (75% yield) of the title compound as a white solid.

後処理

  1. temperatureto reflux overnight
  2. temperatureThe reaction mixture was cooled
  3. customthe volatiles evaporated
  4. customThe residue was partitioned between water and ethyl acetate
  5. washThe organic phase was washed with water and brine
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. customevaporated
  9. customThe solid was chromatographed on silica gel
  10. washeluting with 10% to 50% ethyl acetate

出典と根拠

ORDレコード
ord-cdc7b9fa79ef48afbf4c574dc0816188
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07998993B2

反応ノート

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