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HCID 23369598、化合物 → HCID 10976036、化合物

HRID 1900830
ノート
印刷プレビュー

反応式

HRID 1900830 の反応式
[OH:1][C:2]1[CH:11]=[CH:10][C:9]([CH3:12])=[C:8]2[C:3]=1[CH:4]=[CH:5][C:6](=[O:13])[NH:7]2.[H][H]>C(O)(=O)C.[Pd]>[OH:1][C:2]1[CH:11]=[CH:10][C:9]([CH3:12])=[C:8]2[C:3]=1[CH2:4][CH2:5][C:6](=[O:13])[NH:7]2
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 23369598HCID 23369598、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 10976036HCID 10976036、化合物収率 99.9%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

5-Hydroxy-8-methylcarbostyril (20.0 g, 0.114M) was dissolved in acetic acid (800 ml). To the solution, 10% palladium-on-carbon (10.0 g) was added. The mixture was stirred at 80° C. for 4 hours in the stream of hydrogen. The reaction mixture was filtered, and the filtrate was distilled off under reduced pressure. The residue was extracted from a mixture of chloroform-methanol (10:1) and saturated aqueous sodium bicarbonate solution. The organic phase was washed with saturated aqueous NaCl solution, dried, and condensed under reduced pressure. The resultant residue was recrystallized from methanol-ether to obtain 20.2 g of the title compound as pale yellow powdery crystals (99.9%).

後処理

  1. filtrationThe reaction mixture was filtered
  2. distillationthe filtrate was distilled off under reduced pressure
  3. extractionThe residue was extracted from a mixture of chloroform-methanol (10:1) and saturated aqueous sodium bicarbonate solution
  4. washThe organic phase was washed with saturated aqueous NaCl solution
  5. customdried
  6. customcondensed under reduced pressure
  7. customThe resultant residue was recrystallized from methanol-ether

出典と根拠

ORDレコード
ord-a6026dee68434b418560ec6abe514522
出典データセット
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05576324

反応ノート

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