Hydrochloric Acid → 2-[(4-formyl-1,3-dimethyl-1H-pyrazol-5-yl)sulfanyl]acetic acid

HRID 534817노트

반응식

HRID 534817 반응식
[CH:1]([C:3]1[C:4]([CH3:16])=[N:5][N:6]([CH3:15])[C:7]=1[S:8][CH2:9][C:10]([O:12]CC)=[O:11])=[O:2].[OH-].[Na+].CO.Cl>O1CCCC1>[CH:1]([C:3]1[C:4]([CH3:16])=[N:5][N:6]([CH3:15])[C:7]=1[S:8][CH2:9][C:10]([OH:12])=[O:11])=[O:2]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 63802037Ethyl [(4-formyl-1,3-dimethyl-1H-pyrazol-5-yl)sulfanyl]acetate

생성물 1

HCID 470023932-[(4-formyl-1,3-dimethyl-1H-pyrazol-5-yl)sulfanyl]acetic acid수율 58%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of ethyl [(4-formyl-1,3-dimethyl-1H-pyrazol-5-yl)sulfanyl]acetate obtained in Reference Example 2 (2.12 g), 8 M sodium hydroxide solution (5 mL), methanol (50 mL), and tetrahydrofuran (50 mL) was stirred at room temperature for 2 h. 6 M Hydrochloric acid solution was added to the reaction solution, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was recrystallized from ethyl acetate-diisopropyl ether to provide the title compound (1.09 g, 58%) as a solid.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was recrystallized from ethyl acetate-diisopropyl ether

출처 및 근거

ORD 기록
ord-fd99a6f0705d4451a3c57a118e994a34
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08853215B2

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