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Methanol → 1-(2,6-Difluorobenzyl)-1H-1,2,3-triazole-4-carboxyamide

HRID 218815
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인쇄 미리보기

반응식

HRID 218815 반응식
[F:1][C:2]1[CH:17]=[CH:16][CH:15]=[C:14]([F:18])[C:3]=1[CH2:4][N:5]1[CH:9]=[C:8]([C:10](OC)=O)[N:7]=[N:6]1.[NH4+:19].[OH-:20].[CH3:21]O>O>[F:18][C:14]1[CH:15]=[CH:16][CH:17]=[C:2]([F:1])[C:3]=1[CH2:4][N:5]1[CH:9]=[C:8]([CH2:10][C:21]([NH2:19])=[O:20])[N:7]=[N:6]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 14923Ammonium HydroxideHCID 22716778CGP-47292 methyl ester

생성물 1

HCID 1317297751-(2,6-Difluorobenzyl)-1H-1,2,3-triazole-4-carboxyamide수율 87%

시약·촉매·용매 1

HCID 962Water용매

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온도
20 °C

실험 절차

Methyl 1-(2,6-difluorobenzyl)-1H-1,2,3-triazole-4-carboxylate (II) (10.6 g, 41.9 mmoles), prepared as reported in Example 7, is dissolved in methanol (10 ml) and treated at room temperature under stirring with a 30% ammonia aqueous solution (40 ml), then the reaction mixture is refluxed and kept under stirring for 3 hours. The mixture is cooled to 20° C., then diluted with water, filtered, and the resulting white solid is washed with water and dried in a static dryer at 50° C. Rufinamide (8.7 g) is obtained as a crystalline white solid in 87% yield.

후처리

  1. additiontreated at room temperature
  2. temperaturethe reaction mixture is refluxed
  3. filtrationfiltered
  4. washthe resulting white solid is washed with water
  5. customdried in a static dryer at 50° C

출처 및 근거

ORD 기록
ord-1f9b864bb9044e54a11883ad9405afb8
출처 데이터셋
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08198459B2

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