Styphnic acid → 1,3-Benzenediol, 2,4,6-trinitro-, magnesium salt (1:1)

HRID 1606591Notes

Reaction equation

HRID 1606591 reaction equation
[C:1]1([C:16]([OH:17])=[C:12]([N+:13]([O-:15])=[O:14])[CH:11]=[C:7]([N+:8]([O-:10])=[O:9])[C:5]=1[OH:6])[N+:2]([O-:4])=[O:3].C(=O)([O-])[O-].[Mg+2:22]>O>[C:1]1([C:5]([O-:6])=[C:7]([N+:8]([O-:10])=[O:9])[CH:11]=[C:12]([N+:13]([O-:15])=[O:14])[C:16]=1[O-:17])[N+:2]([O-:4])=[O:3].[Mg+2:22]

Participants

4

Reactant 2

HCID 6721Styphnic acidHCID 11029Magnesium Carbonate

Product 1

HCID 832691,3-Benzenediol, 2,4,6-trinitro-, magnesium salt (1:1)

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
45 °C

Procedure

A magnesium styphnate solution was prepared by the steps of adding 27.5 kg (dry weight) of styphnic acid to 70 liters of distilled water, warming the solution to 45°C, and then adding 11.3 Kg magnesium carbonate (heavy) in small quantities with stirring. The temperature was increased to 55°-60°C and stirring was continued until solution was complete. The solution was cooled, the volume adjusted to 110 liters, filtered and the pH was found to be above 7.2. An analysis of this solution showed that it contained 245g styphnate ion (as styphnic acid) per liter. 330 ml of nitric acid (sp gr 1.42) was then added with stirring.

Workup

  1. temperatureThe temperature was increased to 55°-60°C
  2. stirringstirring
  3. temperatureThe solution was cooled
  4. filtrationfiltered
  5. addition330 ml of nitric acid (sp gr 1.42) was then added
  6. stirringwith stirring

Sources & evidence

ORD record
ord-c77599bbabef4100b99bef6eed02668d
Source dataset
uspto-grants-1976_04
Patent number
US03953486

Reaction notes

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