3(2H)-Pyridazinone, 4,5-dibromo-2-methyl- → 4-Bromo-5-methoxy-2-methylpyridazin-3(2H)-one

HRID 797

반응식

HRID 797 반응식
[Br:1][C:2]1[C:3](=[O:10])[N:4]([CH3:9])[N:5]=[CH:6][C:7]=1Br.[CH3:11][O-:12].[Na+]>CO>[Br:1][C:2]1[C:3](=[O:10])[N:4]([CH3:9])[N:5]=[CH:6][C:7]=1[O:12][CH3:11]

참가 물질

4

반응물 2

HCID 2030123(2H)-Pyridazinone, 4,5-dibromo-2-methyl-HCID 10942334Sodium Methoxide

생성물 1

HCID 106326414-Bromo-5-methoxy-2-methylpyridazin-3(2H)-one

시약·촉매·용매 1

HCID 887Methanol용매2회

반응 조건

온도
23 °C

실험 절차

4,5-Dibromo-2-methyl-3(2H)-pyridazinone (20 g, Maybridge Chemical Company) was cooled in an ice bath and treated successively with methanol (200 mL) and sodium methoxide (12 mL of a 30% solution in methanol). The ice bath was removed and the reaction was allowed to stir at 23° C. for 3 h. The methanol was removed by evaporation at reduced pressure. The residue was partitioned between dichloromethane and water. The organic layer was dried over magnesium sulfate and concentrated to provide the desired product 17 g as a whim solid melting at 146°-147° C. 1 H NMR (CDCl3): 7.7 (1H), 4.0 (3H), 3.8 (3H).

후처리

  1. customThe ice bath was removed
  2. customThe methanol was removed by evaporation at reduced pressure
  3. customThe residue was partitioned between dichloromethane and water
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-9053e57f398646fcad52b73dfd0e8b51
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05723411

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