Ammonium Chloride → HCID 21192057, compound

HRID 1067145Notes

Reaction equation

HRID 1067145 reaction equation
[CH3:1][C:2]1[C:13]([N+:14]([O-])=O)=[C:5]2[N:6]=[C:7]([CH3:12])[C:8]([CH3:11])=[C:9]([CH3:10])[N:4]2[N:3]=1.[Cl-:17].[NH4+]>[Zn].C(O)C>[ClH:17].[CH3:1][C:2]1[C:13]([NH2:14])=[C:5]2[N:6]=[C:7]([CH3:12])[C:8]([CH3:11])=[C:9]([CH3:10])[N:4]2[N:3]=1

Participants

5

Reactant 2

HCID 25517Ammonium ChlorideHCID 21192072HCID 21192072, compound

Product 1

HCID 21192057HCID 21192057, compoundYield 88.3%

Reagents, catalysts & solvents 2

HCID 23994ZincCatalystHCID 702EthanolSolvent

Procedure

2.2 g of 2,5,6,7-tetramethyl-3-nitropyrazolo[1,5-a]pyrimidine, 40 cc of ethanol and 1 g of ammonium chloride were introduced into a 100 ml three-necked round-bottomed flask fitted with a magnetic stirrer, a condenser and a thermometer. The medium was brought to reflux, and 2.5 g of zinc powder were added in small portions in order to maintain the reflux. After 0.5 hour of refluxing, the zinciferous sludges were filtered. The filtrate was concentrated until it crystallized. The crystals were filtered off. Drying under vacuum and over phosphoric anhydride yielded 2 g of 2,5,6,7-tetramethylpyrazolo[1,5-a]pyrimidin-3-ylamine hydrochloride (yield=88.2%).

Workup

  1. customfitted with a magnetic stirrer, a condenser
  2. temperatureto reflux
  3. temperatureto maintain the reflux
  4. temperatureAfter 0.5 hour of refluxing
  5. filtrationthe zinciferous sludges were filtered
  6. concentrationThe filtrate was concentrated until it
  7. customcrystallized
  8. filtrationThe crystals were filtered off
  9. dry with materialDrying under vacuum and over phosphoric anhydride

Sources & evidence

ORD record
ord-21f35b39ea344a76b0f0f21f95052c84
Source dataset
uspto-grants-2001_06
Patent number
US06248137B1

Reaction notes

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