Potassium Carbonate → HCID 86711916, 화합물

HRID 1475222노트

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HRID 1475222 반응식
[CH3:1][C:2]1[NH:6][N:5]=[C:4]([C:7]([NH2:9])=[O:8])[N:3]=1.[Br:10][C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([CH2:17]Br)[CH:12]=1.C([O-])([O-])=O.[K+].[K+]>C1COCC1>[Br:10][C:11]1[CH:12]=[C:13]([CH:14]=[CH:15][CH:16]=1)[CH2:17][N:6]1[C:2]([CH3:1])=[N:3][C:4]([C:7]([NH2:9])=[O:8])=[N:5]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 699793-Bromobenzyl bromideHCID 122201083-Methyl-1H-1,2,4-triazole-5-carboxamide

생성물 1

HCID 86711916HCID 86711916, 화합물수율 26%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
50 °C

실험 절차

To a solution of 5-methyl-1H-1,2,4-triazole-3-carboxamide (2.5 g, 19.8 mmol) and 1-bromo-3-(bromomethyl)benzene (5.45 g, 21.8 mmol) in THF (99 mL), K2CO3 (5.5 g, 39.6 mmol) was added. The mixture was stirred at 50° C. for 18 h, and then the reaction was filtered under vacuum. The solvent was removed under reduced pressure and the crude product was purified on a Biotage pre-packed silica gel column with a gradient of 0% to 20% MeOH:DCM to afford 1-(3-bromobenzyl)-5-methyl-1H-1,2,4-triazole-3-carboxamide (1.5 g, 26%) as a viscous oil. MS (ES+) C11H11BrN4O requires: 294, 296. found: 295, 297 [MH]+(1:1).

후처리

  1. filtrationthe reaction was filtered under vacuum
  2. customThe solvent was removed under reduced pressure
  3. customthe crude product was purified on a Biotage pre-packed silica gel column with a gradient of 0% to 20% MeOH

출처 및 근거

ORD 기록
ord-92d6d784efb24c279acd83764e6f33fa
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09018380B2

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