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Hydrazine hydrate (1:1) → 5,8-Difluorophthalazine-1,4-dione

HRID 382929
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HRID 382929 반응식
[F:1][C:2]1[CH:12]=[CH:11][C:10]([F:13])=[C:4]2[C:5]([O:7][C:8](=O)[C:3]=12)=[O:6].O.O.O.C([O-])(=O)C.[Na+].O.[NH2:23][NH2:24]>C(O)(=O)C>[F:1][C:2]1[CH:12]=[CH:11][C:10]([F:13])=[C:4]2[C:3]=1[C:8](=[O:7])[N:23]=[N:24][C:5]2=[O:6]
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참가 물질

5

반응물 3

HCID 24654Hydrazine hydrate (1:1)HCID 5139183,6-Difluorophthalic anhydrideHCID 23665404Sodium Acetate Trihydrate

생성물 1

HCID 183618865,8-Difluorophthalazine-1,4-dione수율 99.2%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

3,6-Difluorophthalic anhydride (10 g, 54 mmol) was added to a mixture of sodium acetate trihydrate (10 g, 73 mmol) and hydrazine hydrate (5 ml, 156 mmol) in 40% aqueous acetic acid. The reaction was heated under reflux conditions for 16 h and the reaction was filtered to give the title-compound as a white solid (10.5 g, 98%), 1H NMR (250 MHz, d6-DMSO) δ 8.01 (2H, t, J=9 Hz), 11.50-11.80 (2H, br s).

후처리

  1. temperatureThe reaction was heated under reflux conditions for 16 h
  2. filtrationthe reaction was filtered

출처 및 근거

ORD 기록
ord-facc6f27aa704fffa460824878729f9e
출처 데이터셋
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06310203B1

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