Ammonia → HCID 18692760, compound

HRID 1870680Notes

Reaction equation

HRID 1870680 reaction equation
S(=O)(=O)(O)O.Cl.[CH3:7][C:8]1[CH:17]=[C:11]2[N:12]=[CH:13][CH:14]=[C:15]([NH2:16])[N:10]2[N:9]=1.[N+:18]([O-])([OH:20])=[O:19].N>>[CH3:7][C:8]1[C:17]([N+:18]([O-:20])=[O:19])=[C:11]2[N:12]=[CH:13][CH:14]=[C:15]([NH2:16])[N:10]2[N:9]=1

Participants

5

Reactant 4

HCID 222AmmoniaHCID 944Nitric AcidHCID 1118Sulfuric Acid2×HCID 18692763HCID 18692763, compound

Product 1

HCID 18692760HCID 18692760, compoundYield 66%

Procedure

27 cc of 98% sulphuric acid were introduced into a 100 cc three-necked flask equipped with a magnetic stirrer, a thermometer and a condenser, after which 5.5 g of 2-methylpyrazolo[1,5-a]pyrimidin-7-ylamine hydrochloride were dissolved portionwise at 5° C. A mixture of 1.98 g of fuming nitric acid and 5 cc of 98% sulphuric acid was then added dropwise over 30 minutes. After reaction for 2 h 30', the medium was poured onto 200 cc of ice-cold water and neutralized with 122 g of 20% aqueous ammonia. The green precipitate which formed was filtered off. After drying under vacuum over phosphorus pentoxide, 3.8 g of 2-methyl-3-nitropyrazolo[1,5-a]pyrimidin-7-ylamine were obtained in the form of a green powder. (Crude yield=66%).

Workup

  1. customequipped with a magnetic stirrer
  2. additionwas then added dropwise over 30 minutes
  3. customAfter reaction for 2 h 30', the medium
  4. customThe green precipitate which formed
  5. filtrationwas filtered off
  6. dry with materialAfter drying under vacuum over phosphorus pentoxide

Sources & evidence

ORD record
ord-f6d40ce0451444fca3494a2ffb49b597
Source dataset
uspto-grants-2000_08
Patent number
US06099593

Reaction notes

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