Methanol → 2-(4-fluorophenyl)-3-(2-methanesulfonyl-pyrimidin-4-yl)-6,7-dihydro-5H-pyrazolo[1,2-a]pyrazol-1-one

HRID 7639

反応式

HRID 7639 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:15](=[O:16])[N:11]3[CH2:12][CH2:13][CH2:14][N:10]3[C:9]=2[C:17]2[CH:22]=[CH:21][N:20]=[C:19](SC)[N:18]=2)=[CH:4][CH:3]=1.[CH3:25]O.O[O:28][S:29]([O-:31])=O.[K+].S([O-])(O[O-])(=O)=O.[K+].[K+]>C1COCC1.O.C([O-])(O)=O.[Na+]>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:15](=[O:16])[N:11]3[CH2:12][CH2:13][CH2:14][N:10]3[C:9]=2[C:17]2[CH:22]=[CH:21][N:20]=[C:19]([S:29]([CH3:25])(=[O:31])=[O:28])[N:18]=2)=[CH:4][CH:3]=1

参加物

8

反応物 4

HCID 887MethanolHCID 10313463Potassium peroxymonosulphateHCID 129914042-(4-fluorophenyl)-3-(2-methylsulfanyl-pyrimidin-4-yl)-6,7-dihydro-5H-pyrazolo[1,2-a]pyrazol-1-oneHCID 23707502Potassium hydroxy sulfite

生成物 1

HCID 129914052-(4-fluorophenyl)-3-(2-methanesulfonyl-pyrimidin-4-yl)-6,7-dihydro-5H-pyrazolo[1,2-a]pyrazol-1-one

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒HCID 516892Sodium Bicarbonate溶媒

実験手順

To a solution of 2-(4-fluorophenyl)-3-(2-methylsulfanyl-pyrimidin-4-yl)-6,7-dihydro-5H-pyrazolo[1,2-a]pyrazol-1-one, 4, (1.3 g, 3.8 mmol) in THF:methanol (56 mL of a 1:1 mixture) is added dropwise a solution of Oxone® (potassium peroxymonosulfate) (9.34 g, 15.2 mmol) in water (42 mL). The reaction is stirred 1 hour at room temperature, diluted with aqueous NaHCO3 and extract three times with ethyl acetate. The organic layers are combined, dried, and concentrated in vacuo too afford the crude desired product which is used without further purification.

後処理

  1. extractionextract three times with ethyl acetate
  2. customdried
  3. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-245f887f4b944d7aa69c92de847409da
出典データセット
uspto-grants-2006_08
特許番号
US07087615B2

関連ノート

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