Hydrochloric Acid → 1-(5-Methoxy-2-pyridyl)-5-phenylpyrazole-3-carboxylic acid

HRID 1437260노트

반응식

HRID 1437260 반응식
[OH-].[Na+].C([O:5][C:6]([C:8]1[CH:12]=[C:11]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[N:10]([C:19]2[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][N:20]=2)[N:9]=1)=[O:7])C.Cl>CO.O1CCCC1>[CH3:26][O:25][C:22]1[CH:23]=[CH:24][C:19]([N:10]2[C:11]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)=[CH:12][C:8]([C:6]([OH:7])=[O:5])=[N:9]2)=[N:20][CH:21]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 684408421-(5-Methoxy-2-pyridyl)-5-phenylpyrazole-3-carboxylic acid ethyl ester

생성물 1

HCID 230905441-(5-Methoxy-2-pyridyl)-5-phenylpyrazole-3-carboxylic acid수율 94.2%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

Aqueous 1N sodium hydroxide (3.5 mL) was added to the above-obtained 1-(5-methoxy-2-pyridyl)-5-phenylpyrazole-3-carboxylic acid ethyl ester (700 mg) in a mixture of methanol (7 mL) and tetrahydrofuran (7 mL), followed by stirring at room temperature for 2 hours. To the reaction mixture, under cooling with ice, aqueous 1N hydrochloric acid (3.6 mL) was added. The mixture was partitioned between water and ethyl acetate. The organic layer was washed with saturated brine, and then dried over magnesium sulfate anhydrate, followed by filtration. The solvent was removed under reduced pressure, to thereby give the title compound as a solid (602 mg, 94%).

후처리

  1. additionwas added
  2. customThe mixture was partitioned between water and ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over magnesium sulfate anhydrate
  5. filtrationfollowed by filtration
  6. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-ae4243e50d724524983fa8512c615cf1
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07622471B2

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