Diphenyl Ether → 2-Methyl-2,7-dihydro-pyrazolo[3,4-b]pyridin-4-one

HRID 607153ノート

反応式

HRID 607153 の反応式
CC1(C)O[C:6](=[O:8])[C:5](=[CH:9][NH:10][C:11]2[CH:15]=[CH:14][N:13]([CH3:16])[N:12]=2)C(=O)O1.C1(OC2C=CC=CC=2)C=CC=CC=1>CC(C)=O>[CH3:16][N:13]1[CH:14]=[C:15]2[C:11]([NH:10][CH:9]=[CH:5][C:6]2=[O:8])=[N:12]1

参加物

4

反応物 2

HCID 7583Diphenyl EtherHCID 670477842,2-Dimethyl-5-[(1-methyl-1H-pyrazol-3-ylamino)-methylene]-[1,3]dioxane-4,6-dione

生成物 1

HCID 1364007322-Methyl-2,7-dihydro-pyrazolo[3,4-b]pyridin-4-one収率 40.4%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of the product of Example 8a (1.50 g, 5.97 mmol) and diphenyl ether (25 mL) was heated under reflux for 1 h, with removal of the resultant acetone by distillation. The solvent was then decanted, and the remaining solid residue was dissolved in dichloromethane (5 mL) and purified by chromatography on silica gel, eluting with a 0-10% MeOH/CH2Cl2 gradient, to provide the title compound (0.360 g, 40% yield).

後処理

  1. temperaturewas heated
  2. customThe solvent was then decanted
  3. dissolutionthe remaining solid residue was dissolved in dichloromethane (5 mL)
  4. custompurified by chromatography on silica gel
  5. washeluting with a 0-10% MeOH/CH2Cl2 gradient

出典と根拠

ORDレコード
ord-c61d5a4d2d814c71b860c69af59a3f66
出典データセット
uspto-grants-2011_03
特許番号
US07915411B2

反応ノート

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