5-Nitroso-2,4,6-pyrimidinetriamine → tetra-Aminopyrimidine

HRID 1390097Notes

Reaction equation

HRID 1390097 reaction equation
S(O)(O)(=O)=O.[NH2:6][C:7]1[N:12]=[C:11]([NH2:13])[C:10]([NH2:14])=[C:9]([NH2:15])[N:8]=1.N(C1C(N)=NC(N)=NC=1N)=O>O.[Zn]>[NH2:6][C:7]1[N:12]=[C:11]([NH2:13])[C:10]([NH2:14])=[C:9]([NH2:15])[N:8]=1

Participants

5

Reactant 2

HCID 705045-Nitroso-2,4,6-pyrimidinetriamineHCID 79358Tetraaminopyrimidine sulfate

Product 1

HCID 70487tetra-Aminopyrimidine

Reagents, catalysts & solvents 2

HCID 23994ZincCatalystHCID 962WaterSolvent

Procedure

A process for preparing 2,4,5,6-tetraaminopyrimidine sulfate is disclosed. The process comprises: (1) reacting about one molecular proportion of 5-nitroso-2,4,6-triaminopyrimidine (NTAP) in water with about 2.0 to 2.5 molecular proportions of zinc dust and about 4.0 to 4.7 molecular proportions of a suitable acid, to provide a reaction mixture having a pH below 7; (2) reacting the reaction mixture at a temperature of about 20° to 65° C. to form the acid salt of 2,4,5,6-tetraaminopyrimidine; (3) adjusting the pH to about 2.0 to 2.5 by adding the suitable acid to form a solution of the acid salt; (4) separating the insoluble materials from step (3) to obtain a wet cake and a mother liquor; (5) adding sulfuric acid to the mother liquor to adjust the pH to about 0.2 to 0.5 while maintaining the temperature at about 20° to 60° C.; (6) cooling the reaction mixture of step (5) to about 0° to 10° C. to precipitate 2,4,5,6-tetraaminopyrimidine sulfate; and (7) recovering the precipitate.

Workup

  1. customabout 4.0 to 4.7 molecular proportions of a suitable acid, to provide a reaction mixture
  2. customat a temperature of about 20° to 65° C.

Sources & evidence

ORD record
ord-65483ea495fb450685d8487f16200e2d
Source dataset
uspto-grants-1981_01
Patent number
US04247693

Reaction notes

Loading…