Hydrochloric Acid → (2E)-3-(1-methyl-1H-pyrazol-4-yl)prop-2-enoic acid

HRID 30682

반응식

HRID 30682 반응식
[CH3:1][N:2]1[CH:6]=[C:5](/[CH:7]=[CH:8]/[C:9]([O:11]CC)=[O:10])[CH:4]=[N:3]1.CO.[OH-].[Na+].Cl>O1CCCC1>[CH3:1][N:2]1[CH:6]=[C:5](/[CH:7]=[CH:8]/[C:9]([OH:11])=[O:10])[CH:4]=[N:3]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 68356132(E)-Ethyl 3-(1-methyl-1H-pyrazol-4-yl)acrylate

생성물 1

HCID 1529858(2E)-3-(1-methyl-1H-pyrazol-4-yl)prop-2-enoic acid수율 83%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
60 °C

실험 절차

To a mixture of ethyl (2E)-3-(1-methyl-1H-pyrazol-4-yl)acrylate (2.5 g), methanol (20 ml) and tetrahydrofuran (20 ml) was added a 2N aqueous sodium hydroxide solution (13.9 ml) and the mixture was stirred at 60° C. for 3 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 to give (2E)-3-(1-methyl-1H-pyrazol-4-yl)acrylic acid (1.75 g, 83%) as an amorphous form.

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

출처 및 근거

ORD 기록
ord-e3995dd47bdf448cb9568a52cff09b20
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07423159B2

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