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

HRID 872096ノート

反応式

HRID 872096 の反応式
[CH3:1][C:2]1[CH:6]=[C:5]([NH2:7])[NH:4][N:3]=1.[F:8][C:9]1[CH:10]=[C:11]([C:16](=O)[CH2:17][C:18](OCC)=[O:19])[CH:12]=[C:13]([F:15])[CH:14]=1>N1C=CC=CC=1>[F:8][C:9]1[CH:10]=[C:11]([C:16]2[N:4]3[N:3]=[C:2]([CH3:1])[CH:6]=[C:5]3[NH:7][C:18](=[O:19])[CH:17]=2)[CH:12]=[C:13]([F:15])[CH:14]=1

参加物

4

反応物 2

HCID 13550003Ethyl 3-(3,5-difluorophenyl)-3-oxopropanoateHCID 178418690HCID 178418690、化合物

生成物 1

HCID 1363939087-(3,5-difluorophenyl)-2-methylpyrazolo[1,5-a]pyrimidin-5(4H)-one収率 36.8%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

3-Methylpyrazol-5-amine (526 mg) and ethyl 3-(3,5-difluorophenyl)-3-oxopropanoate (879 g) are stirred overnight in a pyridine (30 mL) solvent at 85° 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 (521 mg).

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

出典と根拠

ORDレコード
ord-c43e30d0267e47a992449c85afe83c5a
出典データセット
uspto-grants-2015_03
特許番号
US08975264B2

反応ノート

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