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Hydrochloric Acid → 2-Methoxy-5-(3-methylsulfanyl-[1,2,4]triazol-4-yl)-benzoic acid

HRID 2230744
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반응식

HRID 2230744 반응식
C[O:2][C:3](=[O:19])[C:4]1[CH:9]=[C:8]([N:10]2[CH:14]=[N:13][N:12]=[C:11]2[S:15][CH3:16])[CH:7]=[CH:6][C:5]=1[O:17][CH3:18].[OH-].[Li+].O.Cl>O1CCCC1>[CH3:18][O:17][C:5]1[CH:6]=[CH:7][C:8]([N:10]2[CH:14]=[N:13][N:12]=[C:11]2[S:15][CH3:16])=[CH:9][C:4]=1[C:3]([OH:19])=[O:2]
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 3939Lithium HydroxideHCID 701482672-Methoxy-5-(3-methylsulfanyl-[1,2,4]triazol-4-yl)-benzoic acid methyl ester

생성물 1

HCID 184647022-Methoxy-5-(3-methylsulfanyl-[1,2,4]triazol-4-yl)-benzoic acid수율 95.9%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

실험 절차

Stir a mixture of 2-methoxy-5-(3-methylsulfanyl-[1,2,4]triazol-4-yl)-benzoic acid methyl ester (0.28 g, 3.5 mmol), lithium hydroxide (0.041 g, 3.8 mmol), and 25% water in tetrahydrofuran (20 mL) overnight. Add 1N hydrochloric acid (3.9 mL) dropwise to pH 3. Concentrate to remove the tetrahydrofuran and collect the precipitate by vacuum filtration. Wash the filter cake twice with water and hexane, and dry in vacuo overnight to give 0.89 g of 2-methoxy-5-(3-methylsulfanyl-[1,2,4]triazol-4-yl)-benzoic acid as a solid.

후처리

  1. concentrationConcentrate
  2. customto remove the tetrahydrofuran
  3. customcollect the precipitate
  4. filtrationby vacuum filtration
  5. washWash the filter cake twice with water and hexane
  6. customdry in vacuo overnight

출처 및 근거

ORD 기록
ord-80c074de2c96405881f1ea29644ce28a
출처 데이터셋
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06423704B1

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