Hydrazine hydrate (1:1) → HCID 18361886, compound

HRID 382929Notes

Reaction equation

HRID 382929 reaction equation
[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]

Participants

5

Reactant 3

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

Product 1

HCID 18361886HCID 18361886, compoundYield 99.2%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

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).

Workup

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

Sources & evidence

ORD record
ord-facc6f27aa704fffa460824878729f9e
Source dataset
uspto-grants-2001_10
Patent number
US06310203B1

Reaction notes

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