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Potassium Carbonate → HCID 15005406, 화합물

HRID 1672538
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HRID 1672538 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

HCID 15005406HCID 15005406, 화합물수율 75%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cdc7b9fa79ef48afbf4c574dc0816188
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07998993B2

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