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

HRID 872085

反応式

HRID 872085 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][O:16][C:17]1[CH:18]=[C:19]([C:23](=O)[CH2:24][C:25](OCC)=[O:26])[CH:20]=[CH:21][CH:22]=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:23]([C:19]4[CH:20]=[CH:21][CH:22]=[C:17]([O:16][CH3:15])[CH:18]=4)=[CH:24][C:25](=[O:26])[NH:14][C:5]=23)=[CH:8][CH:9]=1

参加物

4

反応物 2

HCID 2759696Ethyl 3-(3-methoxyphenyl)-3-oxopropanoateHCID 178423836HCID 178423836、化合物

生成物 1

HCID 1364090773-(4-methylphenyl)-7-(3-methoxyphenyl)-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-methoxyphenyl)-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 the target compound is yielded by column chromatography.

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. customthe target compound is yielded by column chromatography

出典と根拠

ORDレコード
ord-2216046163e0473094b17b94538839bb
出典データセット
uspto-grants-2015_03
特許番号
US08975264B2

関連ノート

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