Sodium Bicarbonate → HCID 21449852, compound

HRID 596432Notes

Reaction equation

HRID 596432 reaction equation
[Cl:1]([O-:5])(=[O:4])(=[O:3])=[O:2].[C:6]1([N+:12]2[C:17]([NH2:18])=[C:16](Cl)[C:15]([NH2:20])=[CH:14][N:13]=2)[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.C(=O)(O)[O-].[Na+].[H][H]>[Ni].O>[Cl:1]([O-:5])(=[O:4])(=[O:3])=[O:2].[C:6]1([N+:12]2[C:17]([NH2:18])=[CH:16][C:15]([NH2:20])=[CH:14][N:13]=2)[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1

Participants

6

Reactant 3

HCID 516892Sodium BicarbonateHCID 21449727HCID 21449727, compoundHCID 178418361HCID 178418361, compound

Product 1

HCID 21449852HCID 21449852, compoundYield 76.8%

Reagents, catalysts & solvents 2

HCID 935NickelCatalystHCID 962WaterSolvent

Procedure

32 parts of 1-phenyl-4,6-diamino-5-chloropyridazinium perchlorate in 200 parts of water in a stirred autoclave is stirred with 10 parts of sodium bicarbonate and 2 parts of Raney nickel for 3 hours at 100° C and 200 atmospheres gauge of hydrogen pressure. The discharge is filtered free from nickel and 20 parts of a 70% by weight perchloric acid is added to it. 22 parts (76.8% of theory) of 1-phenyl-4,6-diaminopyridazinium perchlorate is obtained; C10H11O4N4Cl, melting point 105° to 107° C after having been recrystallized from water.

Workup

  1. filtrationThe discharge is filtered free from nickel and 20 parts of a 70% by weight perchloric acid
  2. additionis added to it

Sources & evidence

ORD record
ord-81b26dd1d0584fa69f5803a44e80acd4
Source dataset
uspto-grants-1977_03
Patent number
US04011220

Reaction notes

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