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Hydrochloric Acid → 4-Methyl-1H-1,2,3-triazole-1-acetic acid

HRID 887157
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HRID 887157 반응식
C([O:3][C:4](=[O:12])[CH2:5][N:6]1[CH:10]=[C:9]([CH3:11])[N:8]=[N:7]1)C.CO.[OH-].[Li+].Cl>O1CCCC1>[CH3:11][C:9]1[N:8]=[N:7][N:6]([CH2:5][C:4]([OH:12])=[O:3])[CH:10]=1
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 3939Lithium HydroxideHCID 59603650Ethyl 4-methyl-1H-1,2,3-triazole-1-acetate

생성물 1

HCID 185244434-Methyl-1H-1,2,3-triazole-1-acetic acid수율 95%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 0.51 g (3.0 mmol) of ethyl [4-methyl-1H-1,2,3-triazole-1-yl]acetate from step B above in tetrahydrofuran (10 ml), methanol (6 ml) was added 6 mL (6 mmol) of an aqueous 1.0 M lithium hydroxide solution. The resulting mixture was stirred at ambient temperature for 1 h. The reaction mixture was neutralized with 8 mL of a 2 N hydrochloric acid solution which was then evaporated to remove all volatiles. The aqueous phase was extracted with ethyl acetate and the combined organics were washed with brine, dried over magnesium sulfate, filtered and evaporated to dryness to afford the title compound as a white solid (0.40 g, 95%). LC/MS 142 (M+1).

후처리

  1. customwas then evaporated
  2. customto remove all volatiles
  3. extractionThe aqueous phase was extracted with ethyl acetate
  4. washthe combined organics were washed with brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated to dryness

출처 및 근거

ORD 기록
ord-d916b0d149fe4902b14b554eac15eb2a
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08247415B2

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