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

HRID 80711노트

반응식

HRID 80711 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4b7fb415d5cc49ffbb81e3b61e5f38f4
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846676B2

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