Water → HCID 57285646, compound

HRID 610768Notes

Reaction equation

HRID 610768 reaction equation
S(OOS([O-])(=O)=O)([O-])(=O)=O.[K+].[K+].C([O-])(O)=O.[Na+].[NH2:18][C:19]12[CH:26]3[C:21]4(N)[CH:22]5[C:25]3(N)[CH:24]1[C:23]5(N)[CH:20]24.[O:30]=[O+][O-].[OH2:33]>C(#N)C>[N+:18]([C:19]12[CH:26]3[CH:21]4[CH:22]5[CH:25]3[CH:24]1[CH:23]5[CH:20]24)([O-:30])=[O:33]

Participants

7

Reactant 5

HCID 962Water2×HCID 24412Potassium PersulfateHCID 24823OzoneHCID 516892Sodium BicarbonateHCID 18006654HCID 18006654, compound

Product 1

HCID 57285646HCID 57285646, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

Potassium monopersulfate (6.0 g), NaHCO3 (2.0 g), water (20 ml), and acetonitrile, (30 ml) were mixed together. A solution of the hydrochloride salt of 1,3,5,7-tetraaminocubane in water, 100 mg in 25 ml, was slowly added to the solution while ozone was slowly bubbled through the reaction medium. The reaction temperature was room temperature. The addition of ozone was stopped after 4 hours; the yellowish suspension became milky white. The medium was stirred for 4 days. The reaction product was filtered and the filtrate was concentrated on a rotary evaporator. The concentrate was extracted twice with ethyl acetate (2×50 ml) and washed with aqueous HCl and then with brine. H NMR identified a 1,3,5,7-tetranitrocubane product.

Workup

  1. customwas slowly bubbled through the reaction medium
  2. customwas room temperature
  3. additionThe addition of ozone
  4. filtrationThe reaction product was filtered
  5. concentrationthe filtrate was concentrated on a rotary evaporator
  6. extractionThe concentrate was extracted twice with ethyl acetate (2×50 ml)
  7. washwashed with aqueous HCl

Sources & evidence

ORD record
ord-a7c8a8fb36c7413fafe484ac447c1802
Source dataset
uspto-grants-1999_12
Patent number
US05998661

Reaction notes

Loading…