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

HRID 2230746ノート

反応式

HRID 2230746 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ffbfbe83fb4148829e060adf685ef166
出典データセット
uspto-grants-2002_07
特許番号
US06423704B1

反応ノート

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