Bromoacetone → 6-Chloro-2,8-dimethyl-imidazo[1,2-b]pyridazine

HRID 1946461

반응식

HRID 1946461 반응식
[NH2:1][C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[CH3:8].Br[CH2:11][C:12](=O)[CH3:13]>C(#N)C>[Cl:9][C:5]1[CH:6]=[C:7]([CH3:8])[C:2]2[N:3]([CH:11]=[C:12]([CH3:13])[N:1]=2)[N:4]=1

참가 물질

4

반응물 2

HCID 11715BromoacetoneHCID 123536646-Chloro-4-methylpyridazin-3-amine

생성물 1

HCID 122483406-Chloro-2,8-dimethyl-imidazo[1,2-b]pyridazine

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

3-Amino-6-chloro-4-methylpyridazine (5.50 g, 38.3 mmol) and bromoacetone (6.90 g, 40.0 mmol) were heated in acetonitrile (50.0 ml) for 8 hours under reflux. The reaction solution was concentrated under reduced pressure, and water (100 ml) was added to the residues which were then adjusted to pH 9 with 20% aqueous sodium hydroxide and extracted twice with ethyl acetate. The extracts were combined, dried over anhydrous magnesium sulfate and concentrated, and the residues were purified by silica gel column chromatography (ethyl acetate:chloroform=1:2), to give the title compound as white crystals. The yield was 3.80 g (54.6%).

후처리

  1. temperatureunder reflux
  2. concentrationThe reaction solution was concentrated under reduced pressure, and water (100 ml)
  3. additionwas added to the residues which
  4. extractionextracted twice with ethyl acetate
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customthe residues were purified by silica gel column chromatography (ethyl acetate:chloroform=1:2)

출처 및 근거

ORD 기록
ord-840f21d4cd094b6087ba5b437d42d3bc
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08399381B2

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