Methyl iodide → 1-Methyl-1H-pyrazole-3,5-dicarboxylic acid dimethyl ester

HRID 1256851ノート

反応式

HRID 1256851 の反応式
[CH3:1][O:2][C:3]([C:5]1[CH:9]=[C:8]([C:10]([O:12][CH3:13])=[O:11])[NH:7][N:6]=1)=[O:4].[C:14](=O)([O-])[O-].[K+].[K+].CI>CC(C)=O>[CH3:13][O:12][C:10]([C:8]1[CH:9]=[C:5]([C:3]([O:2][CH3:1])=[O:4])[N:6]([CH3:14])[N:7]=1)=[O:11]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 14844913,5-dimethyl 1H-pyrazole-3,5-dicarboxylate

生成物 1

HCID 125636171-Methyl-1H-pyrazole-3,5-dicarboxylic acid dimethyl ester

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

1H-Pyrazole-3,5-dicarboxylic acid dimethyl ester (639, 9.1 g, 49.0 mmol) was combined with acetone (400 mL) and potassium carbonate (10.2 g, 74.1 mmol). The mixture was stirred for 40 minutes under an atmosphere of nitrogen. To the stirring suspension, methyl iodide (3.4 mL, 54.0 mmol) was added dropwise. The reaction was stirred at room temperature overnight and then the solvent was evaporated under reduced pressure. The resulting solid was washed with water and filtered. After toluene was added, the solvent was removed under reduced pressure. The resulting compound 640 was used without further purification.

後処理

  1. stirringThe reaction was stirred at room temperature overnight
  2. customthe solvent was evaporated under reduced pressure
  3. washThe resulting solid was washed with water
  4. filtrationfiltered
  5. additionAfter toluene was added
  6. customthe solvent was removed under reduced pressure
  7. customThe resulting compound 640 was used without further purification

出典と根拠

ORDレコード
ord-fb1daa1be41f403ca4d04f50a0159bd1
出典データセット
uspto-grants-2013_06
特許番号
US08461169B2

反応ノート

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