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

HRID 720716

반응식

HRID 720716 반응식
C(O[C:4](=[N:6][C:7](=O)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[CH3:5])C.[NH:15]([C:17]1[N:22]=[CH:21][C:20]([S:23]([NH2:26])(=[O:25])=[O:24])=[CH:19][CH:18]=1)[NH2:16].O>ClCCl.CO>[CH3:5][C:4]1[N:6]=[C:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:15]([C:17]2[N:22]=[CH:21][C:20]([S:23]([NH2:26])(=[O:24])=[O:25])=[CH:19][CH:18]=2)[N:16]=1

참가 물질

6

반응물 3

HCID 962WaterHCID 120965903-Pyridinesulfonamide,6-hydrazino-(9CI)HCID 13028604Ethyl (1E)-N-benzoylethanimidate

생성물 1

HCID 98398796-(3-Methyl-5-phenyl-[1,2,4]triazole-1-yl)-pyridine-3-sulfonic acid amide수율 51%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

N-(1-ethoxy-ethylidene)-benzamide 400 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-(3-methyl-5-phenyl-[1,2,4]triazole-1-yl)-pyridine-3-sulfonic acid amide (336 mg, yield: 51%) 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-c057939c297a4774a8e76fa573bc8561
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07135572B2

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