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

HRID 1698541ノート

反応式

HRID 1698541 の反応式
[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

参加物

4

反応物 3

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

生成物 1

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

反応条件

温度
110 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a8c4e69360bb4f4cabe0876abfe53090
出典データセット
uspto-grants-2012_04
特許番号
US08163935B2

反応ノート

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