Nitric Acid → HCID 13755215, compound

HRID 622612Notes

Reaction equation

HRID 622612 reaction equation
[N+:1]([O-:4])(O)=[O:2].[C:5]([NH:9][C:10]1[N:14]([C:15]2[C:20]([Cl:21])=[CH:19][C:18]([Cl:22])=[CH:17][N:16]=2)[N:13]=[CH:12][CH:11]=1)(=[O:8])[CH2:6][CH3:7].C(OC(=O)C)(=O)C>C(O)(=O)C>[C:5]([NH:9][C:10]1[N:14]([C:15]2[C:20]([Cl:21])=[CH:19][C:18]([Cl:22])=[CH:17][N:16]=2)[N:13]=[CH:12][C:11]=1[N+:1]([O-:4])=[O:2])(=[O:8])[CH2:6][CH3:7]

Participants

5

Reactant 3

HCID 944Nitric AcidHCID 7918Acetic AnhydrideHCID 13755214HCID 13755214, compound

Product 1

HCID 13755215HCID 13755215, compoundYield 89%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

1.5 ml (0.033 mole) of 98% strength nitric acid are added to 9.0 g (0.032 mole) of 5-propionamido-1-(3,5-dichloro-pyrid-2-yl)-pyrazole and 3.2 ml (0.035 mole) of acetic anhydride in 35 ml of glacial acetic acid at 10° C. and the mixture is stirred at room temperature for 6 hours. For working up, the mixture is concentrated in vacuo, the residue is taken up in 100 ml of methylene chloride and the mixture is neutralized with sodium bicarbonate solution, washed with sodium chloride solution, dried over magnesium sulphate and freed from the solvent in vacuo. 9.3 g (89% of theory) of 5-propionamido-1-(3,5-dichloropyrid-2-yl)-4-nitro-pyrazole of melting point 53° C.-56° C. are obtained.

Workup

  1. concentrationthe mixture is concentrated in vacuo
  2. washwashed with sodium chloride solution
  3. dry with materialdried over magnesium sulphate

Sources & evidence

ORD record
ord-df48689ba4e74a94a8947db40baa9223
Source dataset
uspto-grants-1988_09
Patent number
US04772312

Reaction notes

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