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

HRID 720722

반응식

HRID 720722 반응식
C(O[C:4](=[N:6][C:7](=O)[C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([F:14])[CH:9]=1)[CH3:5])C.[NH:16]([C:18]1[N:23]=[CH:22][C:21]([S:24]([NH2:27])(=[O:26])=[O:25])=[CH:20][CH:19]=1)[NH2:17].O>ClCCl.CO>[F:14][C:10]1[CH:9]=[C:8]([C:7]2[N:16]([C:18]3[N:23]=[CH:22][C:21]([S:24]([NH2:27])(=[O:26])=[O:25])=[CH:20][CH:19]=3)[N:17]=[C:4]([CH3:5])[N:6]=2)[CH:13]=[CH:12][CH:11]=1

참가 물질

6

반응물 3

HCID 962WaterHCID 120965906-Hydrazinylpyridine-3-sulfonamideHCID 21894666N-(1-ethoxy-ethylidene)-3-fluoro-benzamide

생성물 1

HCID 101934206-[5-(3-Fluoro-phenyl)-3-mehtyl-[1,2,4]triazole-1-yl]-pyridine-3-sulfonic acid amide수율 53.1%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

N-(1-ethoxy-ethylidene)-3-fluoro-benzamide 438 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-(3-fluoro-phenyl)-3-mehtyl-[1,2,4]triazole-1-yl]-pyridine-3-sulfonic acid amide (370 mg, yield: 53%) was obtained as a solid phase.

후처리

  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

출처 및 근거

ORD 기록
ord-23725d2ef6a84069aac5f17ee02c3ee7
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07135572B2

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