Potassium Hydroxide → HCID 178517804, compound

HRID 2389765Notes

Reaction equation

HRID 2389765 reaction equation
[Cl:1][C:2]1[N:7]=[C:6](SC)[N:5]2[N:10]=[CH:11][N:12]=[C:4]2[CH:3]=1.[OH-:13].[K+]>CO>[Cl:1][C:2]1[N:7]=[C:6]([OH:13])[N:5]2[N:10]=[CH:11][N:12]=[C:4]2[CH:3]=1

Participants

4

Reactant 2

HCID 14797Potassium HydroxideHCID 592990517-Chloro-5-methylsulfanyl-[1,2,4]triazolo[1,5-c]pyrimidine

Product 1

HCID 178517804HCID 178517804, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A solution of 2.58 g (12.9 mmol) of 7-chloro-5-(methylthio)[1,2,4]triazolo[1,5-c]pyrimidine (Example 51A) is dissolved in 300 ml of methanol, and 28 ml of a 2 molar aqueous potassium hydroxide solution are added. The mixture is heated under reflux for 3 h. After the reaction is complete, the methanol is removed in vacuo, the mixture is neutralized with half-concentrated hydrochloric acid, and the crystals which have separated out are filtered off with suction. They are washed with water and methanol and then dried under high vacuum. 1.82 g (83% of theory) of the product are obtained.

Workup

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 3 h
  3. customthe methanol is removed in vacuo
  4. customthe crystals which have separated out
  5. filtrationare filtered off with suction
  6. washThey are washed with water and methanol
  7. customdried under high vacuum
  8. custom1.82 g (83% of theory) of the product are obtained

Sources & evidence

ORD record
ord-174a4fc9605d41ceb0b3809fad5dcc41
Source dataset
uspto-grants-2012_09
Patent number
US08273752B2

Reaction notes

Loading…