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

HRID 797

反応式

HRID 797 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
23 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-9053e57f398646fcad52b73dfd0e8b51
出典データセット
uspto-grants-1998_03
特許番号
US05723411

関連ノート

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