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Potassium Carbonate → HCID 86711896, 화합물

HRID 1475200
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HRID 1475200 반응식
[CH3:1][C:2]1[NH:6][N:5]=[C:4]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[N:3]=1.[Cl:12][C:13]1[CH:18]=[C:17]([CH2:19]Cl)[CH:16]=[CH:15][N:14]=1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.O>[Cl:12][C:13]1[CH:18]=[C:17]([CH2:19][N:6]2[C:2]([CH3:1])=[N:3][C:4]([C:7]([O:9][CH2:10][CH3:11])=[O:8])=[N:5]2)[CH:16]=[CH:15][N:14]=1
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6

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HCID 11430Potassium CarbonateHCID 10464537ethyl 3-methyl-1H-1,2,4-triazole-5-carboxylateHCID 111265732-Chloro-4-(chloromethyl)pyridine

생성물 1

HCID 86711896HCID 86711896, 화합물수율 40%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide
용매

실험 절차

To a solution of ethyl 5-methyl-1H-1,2,4-triazole-3-carboxylate (50 mg, 0.28 mmol) and 2-chloro-4-(chloromethyl)pyridine (50 mg, 0.31 mmol) in DMF (2 mL), K2CO3 (116 mg, 0.84 mmol) was added. The mixture was stirred at RT overnight, and was then diluted with H2O (20 mL), extracted with EtOAc (3×20 mL), 4:1 CHCl3:iPrOH (3×20 mL), dried with MgSO4 and concentrated under reduced pressure. The crude product was purified on a Biotage pre-packed silica gel column (EtOAc:Hexane 12% to 100% EtOAc) to afford ethyl 1-((2-chloropyridin-4-yl)methyl)-5-methyl-1H-1,2,4-triazole-3-carboxylate (29 mg, 40%) as a white solid. MS (ES+) C12H13ClN4O2 requires: 280 found: 281[M+H]+.

후처리

  1. extractionextracted with EtOAc (3×20 mL), 4:1 CHCl3
  2. dry with materialiPrOH (3×20 mL), dried with MgSO4
  3. concentrationconcentrated under reduced pressure
  4. customThe crude product was purified on a Biotage pre-packed silica gel column (EtOAc:Hexane 12% to 100% EtOAc)

출처 및 근거

ORD 기록
ord-73c322b85f1b4a689a19d927322851d2
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09018380B2

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