Ammonia → HCID 178513769, compound

HRID 846897Notes

Reaction equation

HRID 846897 reaction equation
[SH:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[N:5]2[N:12]=[CH:13][C:14]([C:15]([O:17]C)=O)=[C:4]2[N:3]=1.[NH3:19]>>[SH:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[N:5]2[N:12]=[CH:13][C:14]([C:15]([NH2:19])=[O:17])=[C:4]2[N:3]=1

Participants

3

Reactant 2

HCID 222AmmoniaHCID 178498899HCID 178498899, compound

Product 1

HCID 178513769HCID 178513769, compound

Procedure

A solution of 1.80 g of methyl 5-mercapto-7-(trifluoromethyl)pyrazolo[1,5-a]pyrimidine-3-carboxylate in 800 ml of 25 percent aqueous ammonia was allowed to stand at 20° for 24 hours. The solution was concentrated to a small volume in a vacuum, made acidic with 1N hydrochloric acid, and extracted with ethyl acetate. The organic phase was washed with saturated sodium chloride solution, dried over sodium sulphate and evaporated in a vacuum. The residual crystal slurry was treated with petroleum ether and filtered. There was obtained 5-mercapto-7-(trifluoromethyl)pyrazolo[1,5-a]pyrimidine-3-carboxamide.

Workup

  1. concentrationThe solution was concentrated to a small volume in a vacuum
  2. extractionextracted with ethyl acetate
  3. washThe organic phase was washed with saturated sodium chloride solution
  4. dry with materialdried over sodium sulphate
  5. customevaporated in a vacuum
  6. additionThe residual crystal slurry was treated with petroleum ether
  7. filtrationfiltered

Sources & evidence

ORD record
ord-e7a48bacf4144d3597950facce67ca11
Source dataset
uspto-grants-1992_08
Patent number
US05138066

Reaction notes

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