Hydrochloric Acid → 3-(1,5-Dimethyl-1H-pyrazol-4-yl)-2-propenoic acid

HRID 30680노트

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HRID 30680 반응식
[CH3:1][N:2]1[C:6]([CH3:7])=[C:5](/[CH:8]=[CH:9]/[C:10]([O:12]CC)=[O:11])[CH:4]=[N:3]1.[OH-].[Na+].Cl>CO>[CH3:1][N:2]1[C:6]([CH3:7])=[C:5](/[CH:8]=[CH:9]/[C:10]([OH:12])=[O:11])[CH:4]=[N:3]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 83766845ethyl (2E)-3-(1,5-dimethyl-1H-pyrazol-4-yl)acrylate

생성물 1

HCID 53740613-(1,5-Dimethyl-1H-pyrazol-4-yl)-2-propenoic acid수율 87%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
60 °C

실험 절차

To a mixture of ethyl (2E)-3-(1,5-dimethyl-1H-pyrazol-4-yl)acrylate (380 mg) and methanol (20 ml) was added a 2N aqueous sodium hydroxide solution (2.0 ml), and the mixture was stirred at 60° C. for 14 hrs. 1N Hydrochloric acid was poured into the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous magnesium sulfate, and concentrated. Recrystallization of the residue from ethyl acetate-hexane gave (2E)-3-(1,5-dimethyl-1H-pyrazol-4-yl)acrylic acid (283 mg, 87%) as colorless prism crystals. melting point: 217-219° C.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customRecrystallization of the residue from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-91129ba6995c4c1d98c84d0f73224267
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07423159B2

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