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Dimethylformamide → 3-(1-Methyl-3-methoxycarbonyl-2-oxo-1,2-dihydropyridin-5-yl)-2-phenylpyrazolo[1,5-a]pyridine

HRID 703996
ノート
印刷プレビュー

反応式

HRID 703996 の反応式
[C:1]([C:4]1C(=O)NC=[C:8]([C:10]2[C:11]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[N:12][N:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=23)[CH:9]=1)([OH:3])=[O:2].[OH-].[K+].[CH3:28]I.[CH3:30][N:31]([CH3:34])[CH:32]=[O:33]>O>[CH3:30][N:31]1[CH:34]=[C:8]([C:10]2[C:11]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[N:12][N:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=23)[CH:9]=[C:4]([C:1]([O:3][CH3:28])=[O:2])[C:32]1=[O:33]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 14797Potassium HydroxideHCID 151581293-(3-Carboxy-2-oxo-1,2-dihydropyridin-5-yl)-2-phenylpyrazolo[1,5-a]pyridine

生成物 1

HCID 151581623-(1-Methyl-3-methoxycarbonyl-2-oxo-1,2-dihydropyridin-5-yl)-2-phenylpyrazolo[1,5-a]pyridine

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

反応条件

温度
2.5 °C

実験手順

To a mixture of 3-(3-carboxy-2-oxo-1,2-dihydropyridin-5-yl)-2-phenylpyrazolo[1,5-a]pyridine (0.92 g) and potassium hydroxide powder (0.54 g) in N,N-dimethylformamide (9 ml) was added 93% methyl iodide (0.64 ml) under ice-cooling (0-5° C.) The mixture was stirred for 3 hours under ice-cooling, and then at room temperature for 1 hour and diluted with water. The resultant precipitates were filtered off and the filtrate was acidified with 5% hydrochloric acid and extracted with ethyl acetate (20 ml). The extract was washed with water (5 ml) and sodium chloride aqueous solution (5 ml), then dried over magnesium sulfate. The solvent was removed and the residue was chromatographed on silica gel (12 g) with a mixture of chloroform and methanol (100:1) as an eluent. The fractions containing the object compound were combined and evaporated in vacuo to give 3-(1-methyl-3-methoxycarbonyl-2-oxo-1,2-dihydropyridin-5-yl)-2-phenylpyrazolo[1,5-a]pyridine (0.34 g).

後処理

  1. temperaturecooling
  2. waitat room temperature for 1 hour
  3. customThe resultant precipitates
  4. filtrationwere filtered off
  5. extractionextracted with ethyl acetate (20 ml)
  6. washThe extract was washed with water (5 ml) and sodium chloride aqueous solution (5 ml)
  7. dry with materialdried over magnesium sulfate
  8. customThe solvent was removed
  9. customthe residue was chromatographed on silica gel (12 g) with a mixture of chloroform and methanol (100:1) as an eluent
  10. additionThe fractions containing the object compound
  11. customevaporated in vacuo

出典と根拠

ORDレコード
ord-52f070dffdac4c96ad6baffcdca5940f
出典データセット
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04985444

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート