Water → 7-bromo-2-chloro-1-methyl-1H-1,3-benzodiazole

HRID 1698541노트

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HRID 1698541 반응식
[Br:1][C:2]1[C:7]2[N:8]([CH3:12])[C:9](=O)[NH:10][C:6]=2[CH:5]=[CH:4][CH:3]=1.O.P(Cl)(Cl)([Cl:16])=O>>[Br:1][C:2]1[C:7]2[N:8]([CH3:12])[C:9]([Cl:16])=[N:10][C:6]=2[CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 3

HCID 962WaterHCID 24813Phosphorus oxychlorideHCID 596354707-bromo-1-methyl-1,3-dihydro-2H-benzimidazol-2-one

생성물 1

HCID 672731127-bromo-2-chloro-1-methyl-1H-1,3-benzodiazole

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온도
110 °C

실험 절차

7-Bromo-1-methyl-1,3-dihydro-2H-benzimidazol-2-one (2.20 g, 9.69 mmol) was dissolved in 30 mL of phosphorous oxychloride and the mixture was heated at 110° C. for 2 days. The reaction allowed to cool to room temperature, poured into water with an ice, and stirred for 1 h. The aqueous solution was extracted with ethyl acetate. The extract was washed with aqueous sodium bicarbonate, dried over magnesium sulfate, filtered and concentrated in vacuo to give 2.32 g of the title compound, which was used in the next reaction without further purification.

후처리

  1. temperatureto cool to room temperature
  2. extractionThe aqueous solution was extracted with ethyl acetate
  3. washThe extract was washed with aqueous sodium bicarbonate
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-a8c4e69360bb4f4cabe0876abfe53090
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08163935B2

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