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Potassium Hydroxide → HCID 70817365, 화합물

HRID 82217
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HRID 82217 반응식
[OH-].[K+].[Cl:3][C:4]1[CH:12]=[C:11]2[C:7]([C:8]([CH2:14][C:15]([O:17]CC)=[O:16])=[N:9][N:10]2[CH3:13])=[CH:6][CH:5]=1>CO>[Cl:3][C:4]1[CH:12]=[C:11]2[C:7]([C:8]([CH2:14][C:15]([OH:17])=[O:16])=[N:9][N:10]2[CH3:13])=[CH:6][CH:5]=1
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참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 70847731Ethyl (6-chloro-1-methyl-1H-indazol-3-yl)acetate

생성물 1

HCID 70817365HCID 70817365, 화합물수율 56%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
25 °C

실험 절차

Aqueous potassium hydroxide (5.93 mL, 10%) was added to ethyl (6-chloro-1-methyl-1H-indazol-3-yl)acetate (Preparation 169, 1.78 g, 0.704 mol) in MeOH (30 mL). The mixture was stirred for 1 hour at 25° C. then the methanol was evaporated in vacuo. The aqueous residue was washed with diethyl ether (30 mL) then acidified with aqueous HCl (6 M). The mixture was extracted with ethyl acetate (30 mL) and the organic phase was dried over sodium sulphate, evaporated in vacuo and purified by column chromatography on silica gel (DCM:MeOH 95:5) to afford the title compound as a white solid in 56% yield, 865 mg.

후처리

  1. customthe methanol was evaporated in vacuo
  2. washThe aqueous residue was washed with diethyl ether (30 mL)
  3. extractionThe mixture was extracted with ethyl acetate (30 mL)
  4. dry with materialthe organic phase was dried over sodium sulphate
  5. customevaporated in vacuo
  6. custompurified by column chromatography on silica gel (DCM:MeOH 95:5)

출처 및 근거

ORD 기록
ord-26182695954a45acb00e1e49a0ed6aaf
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08846698B2

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