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Lithium Hydroxide → 2-Chloro-4-(3-methyl-1H-pyrazol-1-yl)benzoic acid

HRID 2307383
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반응식

HRID 2307383 반응식
C[O:2][C:3](=[O:17])[C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH:14]=[CH:13][C:12]([CH3:15])=[N:11]2)=[CH:6][C:5]=1[Cl:16].[OH-].[Li+]>O1CCCC1>[Cl:16][C:5]1[CH:6]=[C:7]([N:10]2[CH:14]=[CH:13][C:12]([CH3:15])=[N:11]2)[CH:8]=[CH:9][C:4]=1[C:3]([OH:17])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 10634466Methyl 2-chloro-4-(3-Methyl-1H-pyrazol-1-yl)benzoate

생성물 1

HCID 108474542-Chloro-4-(3-methyl-1H-pyrazol-1-yl)benzoic acid수율 78.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 2-chloro-4-(3-methyl-1H-pyrazol-1-yl)-benzoic acid methyl ester (1.42 g) from Example 96 and 6 ml of 1 M aqueous lithium hydroxide in tetrahydrofuran (20 ml) was stirred for 18 hours at room temperature. The reaction mixture was partitioned between ethyl acetate and 1 N hydrochloric acid. The organic layer was washed with water, brine and was dried over anhydrous sodium sulfate. Evaporation of the solvent in vacuo afforded 1.05 g of the title compound as a colorless solid. m.p. 192-193° C. MS (EI), m/z: 236/238 (M)+.

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후처리

  1. customThe reaction mixture was partitioned between ethyl acetate and 1 N hydrochloric acid
  2. washThe organic layer was washed with water, brine
  3. dry with materialwas dried over anhydrous sodium sulfate
  4. customEvaporation of the solvent in vacuo

출처 및 근거

ORD 기록
ord-f5027f06e4d7484390400bf7a9bb2398
출처 데이터셋
uspto-grants-2004_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06831079B1

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