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Hydrazine → HCID 58504230, 화합물

HRID 2407687
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HRID 2407687 반응식
[Cl:1][C:2]1[C:7]2[C:8]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)=[N:9][O:10][C:6]=2[C:5](Cl)=[N:4][N:3]=1.[NH2:18][NH2:19]>O1CCOCC1.C(O)C>[Cl:1][C:2]1[C:7]2[C:8]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)=[N:9][O:10][C:6]=2[C:5]([NH:18][NH2:19])=[N:4][N:3]=1
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참가 물질

5

반응물 2

HCID 9321HydrazineHCID 86659056HCID 86659056, 화합물

생성물 1

HCID 58504230HCID 58504230, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 312751,4-Dioxane용매

실험 절차

To 4,7-dichloro-3-phenylisoxazolo[4,5-d]pyridazine (25.5 g, Desimoni, G.; Et al. Tetrahedron 1967, 23, 681) in 1,4-dioxane (200 mL) and ethanol (50 mL) at 0° C. was added hydrazine (7.0 g) slowly. The reaction mixture was allowed to slowly warm to room temperature. After 20 hours, the reaction mixture was concentrated and the solid obtained was washed with water and filtered. The material was purified by column chromatography on silica gel (methanol:dichloromethane=5:95) to afford first the regioisomer of the title compound followed by the later eluting title compound (4.50 g) having the following physical data.

후처리

  1. concentrationthe reaction mixture was concentrated
  2. customthe solid obtained
  3. washwas washed with water
  4. filtrationfiltered
  5. customThe material was purified by column chromatography on silica gel (methanol:dichloromethane=5:95)

출처 및 근거

ORD 기록
ord-1d73331f422b4bd2ac43d6a2511c8918
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08809538B2

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