Water → 6-[5-(4-Methoxy-phenyl)-3-mehtyl-[1,2,4]triazole-1-yl]-pyridine-3-sulfonic acid amide

HRID 720721ノート

反応式

HRID 720721 の反応式
C(O[C:4](=[N:6][C:7](=O)[C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=1)[CH3:5])C.[NH:17]([C:19]1[N:24]=[CH:23][C:22]([S:25]([NH2:28])(=[O:27])=[O:26])=[CH:21][CH:20]=1)[NH2:18].O>ClCCl.CO>[CH3:15][O:14][C:11]1[CH:10]=[CH:9][C:8]([C:7]2[N:17]([C:19]3[N:24]=[CH:23][C:22]([S:25]([NH2:28])(=[O:27])=[O:26])=[CH:21][CH:20]=3)[N:18]=[C:4]([CH3:5])[N:6]=2)=[CH:13][CH:12]=1

参加物

6

反応物 3

HCID 962WaterHCID 120965906-Hydrazinylpyridine-3-sulfonamideHCID 21894685N-(1-ethoxy-ethylidene)-4-methoxy-benzamide

生成物 1

HCID 102154216-[5-(4-Methoxy-phenyl)-3-mehtyl-[1,2,4]triazole-1-yl]-pyridine-3-sulfonic acid amide収率 55%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

N-(1-ethoxy-ethylidene)-4-methoxy-benzamide 462 mg (2.09 mmol) was dissolved in a mixed solvent of dichloromethane 20 ml and methanol 10 ml, and 6-hydrazinopyridine-3-sulfonic acid amide 433 mg (2.23 mmol) was added to the solution and stirred for 8 hours. After completing the reaction, water 20 ml was added to the reacting solution and extracted two times with dichloromethane, and then, the collected organic layer was washed with saturated brine. The organic layer was dried with anhydrous magnesium sulfate, filtered and concentrated under reduced pressure, and the resulting product was re-crystallized in acetone and hexane phase. As a result, 6-[5-(4-methoxy-phenyl)-3-mehtyl-[1,2,4]triazole-1-yl]-pyridine-3-sulfonic acid amide (397 mg, yield: 55%) was obtained as a solid phase.

後処理

  1. additionwas added to the solution
  2. additionwas added to the reacting solution
  3. extractionextracted two times with dichloromethane
  4. washthe collected organic layer was washed with saturated brine
  5. dry with materialThe organic layer was dried with anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customthe resulting product was re-crystallized in acetone

出典と根拠

ORDレコード
ord-fd27816efd75423ea50769dba59ae391
出典データセット
uspto-grants-2006_11
特許番号
US07135572B2

反応ノート

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