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Potassium Carbonate → 4-(3-Chloropyrazin-2-yloxy)-N-methoxy-N-methylbenzamide

HRID 887464
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HRID 887464 반응식
[OH:1][C:2]1[CH:13]=[CH:12][C:5]([C:6]([N:8]([O:10][CH3:11])[CH3:9])=[O:7])=[CH:4][CH:3]=1.[Cl:14][C:15]1[C:20](Cl)=[N:19][CH:18]=[CH:17][N:16]=1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[Cl:14][C:15]1[C:20]([O:1][C:2]2[CH:13]=[CH:12][C:5]([C:6]([N:8]([O:10][CH3:11])[CH3:9])=[O:7])=[CH:4][CH:3]=2)=[N:19][CH:18]=[CH:17][N:16]=1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 785752,3-DichloropyrazineHCID 113897574-Hydroxy-N-methoxy-N-methylbenzamide

생성물 1

HCID 593513464-(3-Chloropyrazin-2-yloxy)-N-methoxy-N-methylbenzamide

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 4-hydroxy-N-methoxy-N-methylbenzamide (6.50 g, 35.9 mmol), 2,3-dichloropyrazine (6.95 g, 46.6 mmol), and potassium carbonate (12.40 g, 90 mmol) in acetonitrile (70 mL) was heated at reflux in 18 h. The reaction mixture was cooled, concentrated, taken up in H2O, extracted with EtOAc, dried over MgSO4, concentrated and purified by ISCO (50% EtOAc/Hexanes) to give the titled compound. MS [M+1]: 294.1.

후처리

  1. temperaturewas heated
  2. temperatureat reflux in 18 h
  3. temperatureThe reaction mixture was cooled
  4. concentrationconcentrated
  5. extractionextracted with EtOAc
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated
  8. custompurified by ISCO (50% EtOAc/Hexanes)

출처 및 근거

ORD 기록
ord-491bbca5b8a64a57aae352cbf78a5746
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08247418B2

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