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Sodium Hydroxide → 5-chloro-4-(1-methyl-1H-pyrazol-5-yl)thiophene-2-carboxylic acid

HRID 1845377
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HRID 1845377 반응식
[Cl:1][C:2]1[S:6][C:5]([C:7]([O:9]C)=[O:8])=[CH:4][C:3]=1[C:11]1[N:15]([CH3:16])[N:14]=[CH:13][CH:12]=1.[OH-].[Na+]>C1COCC1.CO>[Cl:1][C:2]1[S:6][C:5]([C:7]([OH:9])=[O:8])=[CH:4][C:3]=1[C:11]1[N:15]([CH3:16])[N:14]=[CH:13][CH:12]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 57826577Methyl 5-chloro-4-(1-methyl-1H-pyrazol-5-yl)thiophene-2-carboxylate

생성물 1

HCID 578263895-chloro-4-(1-methyl-1H-pyrazol-5-yl)thiophene-2-carboxylic acid

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

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온도
50 °C
이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

실험 절차

To a solution of methyl 5-chloro-4-(1-methyl-1H-pyrazol-5-yl)-2-thiophenecarboxylate (0.30 g, 1.17 mmole) in THF (10 mL) and MeOH (10 mL) was added 6N NaOH (5 mL). The reaction solution was heated to 50° C. for 2 hrs. The reaction solution was concentrated under vacuum, made acidic (pH ˜2) with 3N HCl, and extracted with DCM. The organic solution was dried (Na2SO4) and concentrated to a solid (0.22 g) which was used without further purification. LC-MS (ES) m/z=243 (M+H)+.

후처리

  1. concentrationThe reaction solution was concentrated under vacuum
  2. extractionextracted with DCM
  3. dry with materialThe organic solution was dried (Na2SO4)
  4. concentrationconcentrated to a solid (0.22 g) which
  5. customwas used without further purification

출처 및 근거

ORD 기록
ord-1e18add0d1a94c2cb9a4f3f3fcef7b95
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08946278B2

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