Acetic Acid → 5,8-Difluoro-2,3-dihydrophthalazine-1,4-dione

HRID 2361020ノート

反応式

HRID 2361020 の反応式
[F:1][C:2]1[CH:10]=[CH:9][C:8]([F:11])=[C:7]2[C:3]=1[C:4](=O)[O:5][C:6]2=[O:12].C([O-])(=O)C.[Na+].C(O)(=O)C.[NH2:23][NH2:24]>O>[F:1][C:2]1[CH:10]=[CH:9][C:8]([F:11])=[C:7]2[C:3]=1[C:4](=[O:5])[NH:23][NH:24][C:6]2=[O:12]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 9321HydrazineHCID 5139183,6-Difluorophthalic anhydrideHCID 517045Sodium Acetate

生成物 1

HCID 667320095,8-Difluoro-2,3-dihydrophthalazine-1,4-dione

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 4,7-difluoroisobenzofuran-1,3-dione (1.00 g, 5.43 mmol) and sodium acetate (0.535 g, 6.52 mmol) was added water (14 mL), acetic acid (7.15 ml, 125 mmol) and hydrazine (0.205 ml, 6.52 mmol) (slowly). A water condenser was attached and the mixture was heated to reflux for 20 hours. Cooled to RT and filtered the resulting solid. Washed with water and dried to yield 5,8-difluoro-2,3-dihydrophthalazine-1,4-dione as a white solid. MS m/z=199 [M+1]+. Calc'd for C8H4P2N2O2: 198.13.

後処理

  1. customA water condenser was attached
  2. temperaturethe mixture was heated
  3. temperatureto reflux for 20 hours
  4. filtrationfiltered the resulting solid
  5. washWashed with water
  6. customdried

出典と根拠

ORDレコード
ord-284f0cb2912d4b38bb68f7efb6437ae9
出典データセット
uspto-grants-2014_04
特許番号
US08686155B2

反応ノート

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