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Cesium carbonate → HCID 84689554, 화합물

HRID 2406688
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HRID 2406688 반응식
[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Br:8])[CH:7]=1.C(=O)([O-])[O-].[Cs+].[Cs+].CN1CCCC1=O.[NH:22]1[CH:26]=[CH:25][N:24]=[N:23]1>C(OCC)(=O)C.O>[Br:8][C:6]1[CH:5]=[N:4][CH:3]=[C:2]([N:23]2[N:24]=[CH:25][CH:26]=[N:22]2)[CH:7]=1.[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([N:22]2[CH:26]=[CH:25][N:24]=[N:23]2)[CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 10796Cesium carbonateHCID 13387N-methyl-2-pyrrolidoneHCID 693693,5-DibromopyridineHCID 178418936HCID 178418936, 화합물

생성물 2

HCID 84689554HCID 84689554, 화합물HCID 84689556HCID 84689556, 화합물

시약·촉매·용매 2

HCID 962
Water
용매
HCID 8857Ethyl Acetate용매

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온도
100 °C

실험 절차

3,5-dibromopyridine (400 mg) and cesium carbonate (550 mg) were added to an N-methylpyrrolidone (4 ml) solution containing 1H-1,2,3-triazole (117 mg), followed by stirring at 100° C. for 21 hours. The reaction mixture was cooled to room temperature, and water and ethyl acetate were added. The organic layer was collected, washed with water and then with saturated saline, and dried over anhydrous magnesium sulfate, and the solvent was distilled away under reduced pressure. The obtained residue was purified by silica gel chromatography (hexane:ethyl acetate=10:0 to 2:3), and a white solid of 3-bromo-5-(2H-1,2,3-triazol-2-yl)pyridine (55 mg) and a white solid of 3-bromo-5-(1H-1,2,3-triazol-1-yl)pyridine (48 mg) were thus obtained.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customThe organic layer was collected
  3. washwashed with water
  4. dry with materialwith saturated saline, and dried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled away under reduced pressure
  6. customThe obtained residue was purified by silica gel chromatography (hexane:ethyl acetate=10:0 to 2:3)

출처 및 근거

ORD 기록
ord-752d98e730004cb8bde1653063a78559
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08809371B2

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