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

HRID 2230746노트

반응식

HRID 2230746 반응식
C[O:2][C:3](=[O:21])[C:4]1[CH:9]=[C:8]([N:10]2[CH:14]=[N:13][N:12]=[C:11]2[S:15]([CH3:18])(=[O:17])=[O:16])[CH:7]=[CH:6][C:5]=1[O:19][CH3:20].[OH-].[Li+].O.Cl>O1CCCC1>[CH3:18][S:15]([C:11]1[N:10]([C:8]2[CH:7]=[CH:6][C:5]([O:19][CH3:20])=[C:4]([CH:9]=2)[C:3]([OH:21])=[O:2])[CH:14]=[N:13][N:12]=1)(=[O:16])=[O:17]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 3939Lithium HydroxideHCID 701493355-(3-Methanesulfonyl-[1,2,4]triazol-4-yl)-2-methoxy-benzoic acid methyl ester

생성물 1

HCID 184644745-(3-Methanesulfonyl-[1,2,4]triazol-4-yl)-2-methoxy-benzoic acid수율 83%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Stir a mixture of 5-(3-methanesulfonyl-[1,2,4]triazol-4-yl)-2-methoxy-benzoic acid methyl ester (1.0 g, 3.2 mmol), lithium hydroxide (0.042 g, 3.6 mmol), and 25% water in tetrahydrofuran (30 mL) at reflux overnight. Cool and add 1N hydrochloric acid (3.6 mL) dropwise via syringe. 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 0.79 g of 5-(3-methanesulfonyl-[1,2,4]triazol-4-yl)-2-methoxy-benzoic acid as a solid.

후처리

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

출처 및 근거

ORD 기록
ord-ffbfbe83fb4148829e060adf685ef166
출처 데이터셋
uspto-grants-2002_07
특허 번호
US06423704B1

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