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

HRID 607153노트

반응식

HRID 607153 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c61d5a4d2d814c71b860c69af59a3f66
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07915411B2

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