Pyridazine-4-carboxylic Acid → 3-Methylpyridazine-4-carboxylic acid
反応式
[N:1]1[CH:6]=[CH:5][C:4]([C:7]([OH:9])=[O:8])=[CH:3][N:2]=1.CO.[CH2:12](Cl)Cl>>[CH3:12][C:3]1[N:2]=[N:1][CH:6]=[CH:5][C:4]=1[C:7]([OH:9])=[O:8]参加物
3
実験手順
To a solution of 4-pyridazinecarboxylic acid (490 mg, 3.9 mmol) in MeOH/DCM (20/10 ml) was added at 0° C. trimethylsilildiazomethane (25.5 mmol). The solution was warm at r.t. and stirred overnight. Volatiles were evaporated in vacuo, the crude dissolved in DCM, washed with NaHCO3 satured and dried over Na2SO4. After filtration and concentration to dryness in vacuo, the crude was purified by column chromatography (DCM:MeOH=98 to 2) to give 400 mg of the title compound.
後処理
- customVolatiles were evaporated in vacuo
- dissolutionthe crude dissolved in DCM
- washwashed with NaHCO3
- dry with materialdried over Na2SO4
- filtrationAfter filtration and concentration to dryness in vacuo
- customthe crude was purified by column chromatography (DCM:MeOH=98 to 2)
出典と根拠
- ORDレコード
- ord-3350765f503146e58941656a0524ca59
- 出典データセット
- uspto-grants-2011_05
- 特許番号
- US07947683B2
反応ノート
読み込み中…