Hydrochloric Acid → HCID 18692763, compound

HRID 1870679Notes

Reaction equation

HRID 1870679 reaction equation
[ClH:1].[NH2:2][C:3]1[CH:7]=[C:6]([CH3:8])[NH:5][N:4]=1.C(O[CH:12]=[CH:13][C:14]#[N:15])C>O>[ClH:1].[CH3:8][C:6]1[CH:7]=[C:3]2[N:2]=[CH:12][CH:13]=[C:14]([NH2:15])[N:4]2[N:5]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 436013-Ethoxy-2-propenenitrileHCID 931461H-Pyrazol-3-amine, 5-methyl-

Product 1

HCID 18692763HCID 18692763, compoundYield 83%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

150 cc of 35% hydrochloric acid were introduced into a 500 cc three-necked flask equipped with a magnetic stirrer, a thermometer and a condenser, and 47.5 g of 3-amino-5-methylpyrazole dissolved in 100 cc of water were added dropwise. The temperature rose to 60° C. 47.5 g of 3-ethoxyacrylonitrile were then added and the reaction was refluxed for 1 h. The reaction medium was cooled and concentrated under reduced pressure. 50 cc of acetone were added and the precipitate obtained was filtered off. It was rinsed with diisopropyl ether. After drying under vacuum over phosphorus pentoxide, 78.7 g of 2-methylpyrazolo[1,5-a]pyrimidin-7-ylamine hydrochloride were obtained in the form of white crystals. (Yield=83%).

Workup

  1. customequipped with a magnetic stirrer
  2. additionwere added dropwise
  3. customrose to 60° C
  4. temperaturethe reaction was refluxed for 1 h
  5. temperatureThe reaction medium was cooled
  6. concentrationconcentrated under reduced pressure
  7. addition50 cc of acetone were added
  8. customthe precipitate obtained
  9. filtrationwas filtered off
  10. washIt was rinsed with diisopropyl ether
  11. dry with materialAfter drying under vacuum over phosphorus pentoxide

Sources & evidence

ORD record
ord-682c40730956465a9cb8c7bd6b9df770
Source dataset
uspto-grants-2000_08
Patent number
US06099593

Reaction notes

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