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

HRID 22678

反応式

HRID 22678 の反応式
[CH3:1][N:2]([CH3:27])[CH:3]1[CH2:7][N:6]2[C:8](=[O:26])[C:9]([C:19]3[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=3)=[C:10]([C:11]3[CH:16]=[CH:15][N:14]=[C:13](SC)[N:12]=3)[N:5]2[CH2:4]1.[CH3:28]O.O[O:31][S:32]([O-:34])=O.[K+].S([O-])(O[O-])(=O)=O.[K+].[K+]>C1COCC1.O.C([O-])(O)=O.[Na+]>[CH3:27][N:2]([CH3:1])[CH:3]1[CH2:7][N:6]2[C:8](=[O:26])[C:9]([C:19]3[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=3)=[C:10]([C:11]3[CH:16]=[CH:15][N:14]=[C:13]([S:32]([CH3:28])(=[O:34])=[O:31])[N:12]=3)[N:5]2[CH2:4]1

参加物

8

反応物 4

HCID 887MethanolHCID 10313463Potassium peroxymonosulphateHCID 219922076-dimethylamino-2-(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 219922086-dimethylamino-2-(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 6-dimethylamino-2-(4-fluorophenyl)-3-(2-methylsulfanyl-pyrimidin-4-yl)-6,7-dihydro-5H-pyrazolo[1,2-a]pyrazol-1-one, 24, (3.9 g, 10 mmol) in THF:methanol (150 mL of a 1:1 mixture) is added dropwise a solution of Oxone® (potassium peroxymonosulfate) (24.3 g, 39.5 mmol) in water (100 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 to 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-a86e3a986d9d48189cb721c80156fa5b
出典データセット
uspto-grants-2005_02
特許番号
US06849627B2

関連ノート

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