Hydrochloric Acid → [1-(4-Chlorophenyl)-5-methyl-1H-pyrazol-4-yl]methanol

HRID 1603747노트

반응식

HRID 1603747 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12]([CH3:13])=[C:11]([C:14](OCC)=[O:15])[CH:10]=[N:9]2)=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].Cl>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[C:12]([CH3:13])=[C:11]([CH2:14][OH:15])[CH:10]=[N:9]2)=[CH:6][CH:7]=1

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 4282610ethyl 1-(4-chlorophenyl)-5-methyl-1H-pyrazole-4-carboxylateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 19606233[1-(4-Chlorophenyl)-5-methyl-1H-pyrazol-4-yl]methanol수율 91%

실험 절차

To a solution of 3.2 g of ethyl 1-(4-chlorophenyl)-5-methyl-1H-pyrazole-4-carboxylate, 0.46 g of lithium aluminum hydride was added, followed by stirring for 1.5 hours at room temperature. The reaction mixture was added with a 5% aqueous solution of hydrochloric acid and then extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium chloride, dried over magnesium sulfate and then filtered. The filtrate was concentrated under reduced pressure. The residue was subjected to chromatography on a silica gel column and then purified using gradient elution with hexane-ethyl acetate, whereby 2.45 g of the title compound were obtained (yield: 91%).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with an aqueous solution of sodium chloride
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated under reduced pressure
  6. custompurified
  7. washelution with hexane-ethyl acetate

출처 및 근거

ORD 기록
ord-c513e356f51a43ee8eda8cfaab6c0b36
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05990139

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