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

HRID 872096노트

반응식

HRID 872096 반응식
[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

참가 물질

4

반응물 2

HCID 13550003Ethyl 3-(3,5-difluorophenyl)-3-oxopropanoateHCID 178418690HCID 178418690, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c43e30d0267e47a992449c85afe83c5a
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08975264B2

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