Hydrochloric Acid → HCID 131713500, compound

HRID 543505Notes

Reaction equation

HRID 543505 reaction equation
[F:1][CH:2]([F:30])[CH:3]([N:19]1C(=O)C2=CC=CC=C2C1=O)[CH2:4][C:5](=[CH2:18])[CH2:6][N:7]1C(=O)C2=CC=CC=C2C1=O.O.NN.O.[ClH:35]>C(O)C>[ClH:35].[ClH:35].[F:1][CH:2]([F:30])[CH:3]([NH2:19])[CH2:4][C:5](=[CH2:18])[CH2:6][NH2:7]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 20461671HCID 20461671, compound

Product 1

HCID 131713500HCID 131713500, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
90 °C

Procedure

A mixture of 1,1-difluoro-2,5-diphthalimido-4-methylene-pentane (7.77 g, 19 mmoles) prepared as in Step D above, and hydrazine hydrate (38 mL of a 1 M solution in ethanol) is heated for 5 hours at 90° C. After addition of water (30 mL) and concentrated hydrochloric acid (60 mL) heating is continued for one more hour at 90° C. After filtration, and evaporation to dryness, the residue is dissolved in water, and the remaining phthalhydrazide is elimated by filtration. Concentration under vacuum affords an oil which is used without further purification.

Workup

  1. temperatureheating
  2. customis continued for one more hour at 90° C
  3. filtrationAfter filtration, and evaporation to dryness
  4. dissolutionthe residue is dissolved in water
  5. filtrationthe remaining phthalhydrazide is elimated by filtration
  6. concentrationConcentration under vacuum
  7. customaffords an oil which
  8. customis used without further purification

Sources & evidence

ORD record
ord-edee0fa0dac5404cb6ac73dc6b16ca05
Source dataset
uspto-grants-1984_05
Patent number
US04446151

Reaction notes

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