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Hydrochloric Acid → (2E)-3-[5-(3-furyl)-1-methyl-1H-pyrazol-4-yl]acrylic acid

HRID 30675
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인쇄 미리보기

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HRID 30675 반응식
[O:1]1[CH:5]=[CH:4][C:3]([C:6]2[N:10]([CH3:11])[N:9]=[CH:8][C:7]=2/[CH:12]=[CH:13]/[C:14]([O:16]CC)=[O:15])=[CH:2]1.O1CCCC1.[OH-].[Na+].Cl>C(O)C>[O:1]1[CH:5]=[CH:4][C:3]([C:6]2[N:10]([CH3:11])[N:9]=[CH:8][C:7]=2/[CH:12]=[CH:13]/[C:14]([OH:16])=[O:15])=[CH:2]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 86602517HCID 86602517, 화합물

생성물 1

HCID 69209210(2E)-3-[5-(3-furyl)-1-methyl-1H-pyrazol-4-yl]acrylic acid수율 99.2%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
60 °C

실험 절차

To a mixture of ethyl (2E)-3-[5-(3-furyl)-1-methyl-1H-pyrazol-4-yl]acrylate (800 mg), tetrahydrofuran (10 ml) and ethanol (10 ml) was added 2N aqueous sodium hydroxide solution (6.5 ml) and the mixture was stirred at 60° C. for 1 hr. 1N Hydrochloric acid was poured into the reaction mixture, and the precipitated solids were collected by filtration, washed with water and dried with airflow to give (2E)-3-[5-(3-furyl)-1-methyl-1H-pyrazol-4-yl]acrylic acid (703 mg, 99%) as crystals. Recrystallization thereof from ethyl acetate-hexane gave colorless prism crystals. melting point: 218-219° C.

후처리

  1. filtrationthe precipitated solids were collected by filtration
  2. washwashed with water
  3. customdried with airflow

출처 및 근거

ORD 기록
ord-c9dc05cf6a3144948feefc6ef2ddbd7a
출처 데이터셋
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07423159B2

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