Pyridazine-4-carboxylic Acid → 3-Methylpyridazine-4-carboxylic acid

HRID 550528

反応式

HRID 550528 の反応式
[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

反応物 2

HCID 2761046Pyridazine-4-carboxylic AcidHCID 21226129Dichloromethane methanol

生成物 1

HCID 534147303-Methylpyridazine-4-carboxylic acid

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

  1. customVolatiles were evaporated in vacuo
  2. dissolutionthe crude dissolved in DCM
  3. washwashed with NaHCO3
  4. dry with materialdried over Na2SO4
  5. filtrationAfter filtration and concentration to dryness in vacuo
  6. 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

関連ノート

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