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Butylamine → HCID 47174299, 화합물

HRID 2042716
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HRID 2042716 반응식
[Cl:1][C:2]1[C:3](=[O:10])[N:4]([CH3:9])[N:5]=[CH:6][C:7]=1[Cl:8].[CH2:11]([NH2:15])[CH2:12][CH2:13][CH3:14]>C(#N)C>[CH2:11]([NH:15][C:2]1[C:3](=[O:10])[N:4]([CH3:9])[N:5]=[CH:6][C:7]=1[Cl:8])[CH2:12][CH2:13][CH3:14].[CH2:11]([NH:15][C:7]1[CH:6]=[N:5][N:4]([CH3:9])[C:3](=[O:10])[C:2]=1[Cl:1])[CH2:12][CH2:13][CH3:14]
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참가 물질

5

반응물 2

HCID 8007ButylamineHCID 1204623(2H)-Pyridazinone, 4,5-dichloro-2-methyl-

생성물 2

HCID 47174299HCID 47174299, 화합물HCID 67994474HCID 67994474, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 4,5-dichloro-2-methylpyridazin-3(2H)-one (358 mg, 2 mmol) and butan-1-amine (585 mg, 8 mmol) in acetonitrile was refluxed for 16 hours. The mixture was concentrated under reduced pressure, the residue was dissolved in ethyl acetate, washed with water, brine, dried with MgSO4, filtered, and concentrated. Purification of the residue by chromatography (hexanes-EtOAc 1:1) afforded 170 mg of 4-(butylamino)-5-chloro-2-methylpyridazin-3(2H)-one and 260 mg of 5-(butylamino)-4-chloro-2-methylpyridazin-3(2H)-one. MS (ESI) m/z 215 (M+H)+.

후처리

  1. temperaturewas refluxed for 16 hours
  2. concentrationThe mixture was concentrated under reduced pressure
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. washwashed with water, brine
  5. dry with materialdried with MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customPurification of the residue by chromatography (hexanes-EtOAc 1:1)

출처 및 근거

ORD 기록
ord-a849a6112dd7494a8af507ebf067f005
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08586596B2

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