Sulfuric Acid → 5-Ethylthio-7-phenyl-1,2,4-triazolo[4,3-c]pyrimidine dihydrogen sulfate hydrate

HRID 371385Notes

Reaction equation

HRID 371385 reaction equation
[CH2:1]([S:3][C:4]1[N:9]2[CH:10]=[N:11][N:12]=[C:8]2[CH:7]=[C:6]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[N:5]=1)[CH3:2].[S:19](=[O:23])(=[O:22])([OH:21])[OH:20].C(OCC)C>C(O)C>[OH2:20].[S:19]([OH:23])([OH:22])(=[O:21])=[O:20].[CH2:1]([S:3][C:4]1[N:9]2[CH:10]=[N:11][N:12]=[C:8]2[CH:7]=[C:6]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[N:5]=1)[CH3:2]

Participants

5

Reactant 3

HCID 1118Sulfuric AcidHCID 3283Diethyl EtherHCID 13519876HCID 13519876, compound

Product 1

HCID 202352185-Ethylthio-7-phenyl-1,2,4-triazolo[4,3-c]pyrimidine dihydrogen sulfate hydrate

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 3.6 g of 5-ethylthio-7-phenyl-1,2,4-triazolo[4,3-c]pyrimidine in 100 ml of hot ethanol was added 1.4 g of concentrated sulfuric acid. The mixture was cooled, an equal volume of diethyl ether was added and the precipitate was collected by filtration. The precipitate was recrystallized from a mixture of methanol and diethyl ether to provide 5-ethylthio-7-phenyl-1,2,4-triazolo[4,3-c]pyrimidine dihydrogen sulfate hydrate, m.p. 213°-214° C.

Workup

  1. temperatureThe mixture was cooled
  2. filtrationthe precipitate was collected by filtration
  3. customThe precipitate was recrystallized from a mixture of methanol and diethyl ether

Sources & evidence

ORD record
ord-07153e93072149c697184bd5370b32ba
Source dataset
uspto-grants-1985_07
Patent number
US04532242

Reaction notes

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