2-Bromo-1-(4-fluorophenyl)ethan-1-one → 6-Chloro-2-(4-fluorophenyl)-7,8-dimethylimidazo[1,2-b]pyridazine

HRID 80711ノート

反応式

HRID 80711 の反応式
[NH2:1][C:2]1[N:3]=[N:4][C:5]([Cl:10])=[C:6]([CH3:9])[C:7]=1[CH3:8].Br[CH2:12][C:13]([C:15]1[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=1)=O>C(O)C>[Cl:10][C:5]1[C:6]([CH3:9])=[C:7]([CH3:8])[C:2]2[N:3]([CH:12]=[C:13]([C:15]3[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=3)[N:1]=2)[N:4]=1

参加物

4

反応物 2

HCID 967492-Bromo-1-(4-fluorophenyl)ethan-1-oneHCID 69919433-Amino-6-chloro-4,5-dimethylpyridazine

生成物 1

HCID 593677146-Chloro-2-(4-fluorophenyl)-7,8-dimethylimidazo[1,2-b]pyridazine収率 84%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 13 g (85 mmol) of 3-amino-6-chloro-4,5-dimethylpyridazine and 23 g (107 mmol) of 2-bromo-1-(4-fluorophenyl)ethanone in 130 mL of ethanol is refluxed for 16 hours. After cooling, the solvent is evaporated off under reduced pressure and the residue is taken up in chloroform. The organic phase is washed with diluted aqueous ammonia, dried over sodium sulfate and concentrated under reduced pressure to give a brown solid. This solid is triturated in acetone to give 19.2 g of a beige-colored powder.

後処理

  1. temperatureAfter cooling
  2. customthe solvent is evaporated off under reduced pressure
  3. washThe organic phase is washed with diluted aqueous ammonia
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customto give a brown solid
  7. customThis solid is triturated in acetone

出典と根拠

ORDレコード
ord-4b7fb415d5cc49ffbb81e3b61e5f38f4
出典データセット
uspto-grants-2014_09
特許番号
US08846676B2

反応ノート

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