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Ethyl 3-(3-methylphenyl)-3-oxopropanoate → 3-(4-methylphenyl)-7-(3-methylphenyl)-2-methylpyrazolo[1,5-a]pyrimidin-5(4H)-one

HRID 872108
ノート
印刷プレビュー

反応式

HRID 872108 の反応式
[CH3:1][C:2]1[C:6]([C:7]2[CH:12]=[CH:11][C:10]([CH3:13])=[CH:9][CH:8]=2)=[C:5]([NH2:14])[NH:4][N:3]=1.[CH3:15][C:16]1[CH:17]=[C:18]([C:22](=O)[CH2:23][C:24](OCC)=[O:25])[CH:19]=[CH:20][CH:21]=1>N1C=CC=CC=1>[CH3:13][C:10]1[CH:11]=[CH:12][C:7]([C:6]2[C:2]([CH3:1])=[N:3][N:4]3[C:22]([C:18]4[CH:19]=[CH:20][CH:21]=[C:16]([CH3:15])[CH:17]=4)=[CH:23][C:24](=[O:25])[NH:14][C:5]=23)=[CH:8][CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 2760277Ethyl 3-(3-methylphenyl)-3-oxopropanoateHCID 178423836HCID 178423836、化合物

生成物 1

HCID 1363939043-(4-methylphenyl)-7-(3-methylphenyl)-2-methylpyrazolo[1,5-a]pyrimidin-5(4H)-one

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

3-Methyl-4-(4-methylphenyl)-1H-pyrazol-5-amine and ethyl 3-(3-methylphenyl)-3-oxopropanoate are stirred overnight in a pyridine (10 mL) solvent at 95° C. After cooling to room temperature, the reaction solvent is removed by distillation under reduced pressure. The remainder is extracted with ethyl acetate and water. The extracted organic layer is washed with brine and dehydrated with anhydrous MgSO4. The dehydrated organic layer is distilled under reduced pressure and purified by column chromatography to yield the target compound.

後処理

  1. customthe reaction solvent is removed by distillation under reduced pressure
  2. extractionThe remainder is extracted with ethyl acetate and water
  3. washThe extracted organic layer is washed with brine
  4. distillationThe dehydrated organic layer is distilled under reduced pressure
  5. custompurified by column chromatography
  6. customto yield the target compound

出典と根拠

ORDレコード
ord-53f7821f15b948d8a57669f55007223b
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08975264B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート