Sodium Methoxide → 4-Benzyl-3-bromo-5-methoxy-4H-1,2,4-triazole

HRID 1487985노트

반응식

HRID 1487985 반응식
[CH2:1]([N:8]1[C:12](Br)=[N:11][N:10]=[C:9]1[Br:14])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:15][O-:16].[Na+]>CO>[CH2:1]([N:8]1[C:12]([O:16][CH3:15])=[N:11][N:10]=[C:9]1[Br:14])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 10942334Sodium Methoxide2회HCID 900291814-Benzyl-3,5-dibromo-4H-1,2,4-triazole2회

생성물 1

HCID 900294944-Benzyl-3-bromo-5-methoxy-4H-1,2,4-triazole

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 4-benzyl-3,5-dibromo-4H-1,2,4-triazole (compound 91.2, 3.71 g, 11.7 mmol) in MeOH 15 mL) was added NaOMe (1.26 g, 23.4 mmol) and the mixture was refluxed for 18 hours. The mixture was cooled somewhat and additional NaOMe was added (1.26 g, 23.4 mmol). The mixture was refluxed for an additional 5 hours, then cooled to room temperature, and the solvent was removed under reduced pressure. The residue was dissolved in EtOAc (200 mL) and washed with water (30 mL). The organic layer was dried (MgSO4), filtered and concentrated under reduced pressure to yield 3.13 g (theoretical) of the title compound as a clear oil. m/z (ES+) 269 (M+H)+.

후처리

  1. temperaturethe mixture was refluxed for 18 hours
  2. temperatureThe mixture was cooled somewhat
  3. temperatureThe mixture was refluxed for an additional 5 hours
  4. customthe solvent was removed under reduced pressure
  5. dissolutionThe residue was dissolved in EtOAc (200 mL)
  6. washwashed with water (30 mL)
  7. dry with materialThe organic layer was dried (MgSO4)
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-9629677f5d3e47e58313d0cc01e86d23
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09428502B2

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