4,5-二溴-2-甲基哒嗪-3(2H)-酮 → 4-Bromo-5-methoxy-2-methylpyridazin-3(2H)-one

HRID 797

反应方程式

HRID 797 反应方程式
[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]

参与物

4

反应物 2

HCID 2030124,5-二溴-2-甲基哒嗪-3(2H)-酮HCID 10942334甲醇钠

产物 1

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

试剂、催化剂与溶剂 1

HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂2 次

反应条件

温度
23 °C

实验过程

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).

后处理

  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

来源与证据

ORD记录
ord-9053e57f398646fcad52b73dfd0e8b51
来源数据集
uspto-grants-1998_03
专利号
US05723411

关联笔记

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