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Methyl iodide → ethyl 5-methoxy-1H-pyrazole-3-carboxylate

HRID 1181574
ノート
印刷プレビュー

反応式

HRID 1181574 の反応式
[CH2:1]([O:3][C:4]([C:6]1[CH:10]=[C:9]([OH:11])[NH:8][N:7]=1)=[O:5])[CH3:2].[C:12](=O)([O-])[O-].[Cs+].[Cs+].IC>CN(C)C=O>[CH2:1]([O:3][C:4]([C:6]1[CH:10]=[C:9]([O:11][CH3:12])[NH:8][N:7]=1)=[O:5])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 178469373HCID 178469373、化合物

生成物 1

HCID 178469331ethyl 5-methoxy-1H-pyrazole-3-carboxylate収率 38%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

5-Hydroxy-1H-pyrazole-3-carboxylic acid ethyl ester (300 mg, 1.92 mmol) was dissolved in anhydrous N,N-dimethylformamide (DMF) (35 ml) and cesium carbonate (626 mg, 1.92 mmol) was added. The resulting suspension was treated with iodomethane (120 μl, 273 mg, 1.92 mmol) and stirred for 12 h at room temperature. The reaction mixture was quenched with saturated potassium hydrogen sulfate solution and extracted with ethyl acetate (3×100 ml). The combined organic layers were washed with water (50 ml) and brine (50 ml). The extract was dried over sodium sulfate, evaporated and the crude product was purified by column chromatography on silica gel. Elution with ethyl acetate/n-heptane (1:3) yielded 124 mg (38%) of a white solid.

後処理

  1. customThe reaction mixture was quenched with saturated potassium hydrogen sulfate solution
  2. extractionextracted with ethyl acetate (3×100 ml)
  3. washThe combined organic layers were washed with water (50 ml) and brine (50 ml)
  4. dry with materialThe extract was dried over sodium sulfate
  5. customevaporated
  6. customthe crude product was purified by column chromatography on silica gel
  7. washElution with ethyl acetate/n-heptane (1:3)

出典と根拠

ORDレコード
ord-c81f16c948c749b3a200bd8f09761682
出典データセット
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07285569B2

反応ノート

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