Sodium hydrosulfide → HCID 178429722, compound

HRID 973812Notes

Reaction equation

HRID 973812 reaction equation
Cl[C:2]1[N:7]2[N:8]=[C:9]([C:11]([O:13]C)=[O:12])[N:10]=[C:6]2[N:5]=[C:4]([CH3:15])[CH:3]=1.[SH-:16].[Na+]>O>[C:11]([C:9]1[N:10]=[C:6]2[N:5]=[C:4]([CH3:15])[CH:3]=[C:2]([SH:16])[N:7]2[N:8]=1)([OH:13])=[O:12]

Participants

4

Reactant 2

HCID 28015Sodium hydrosulfideHCID 13562758Methyl 7-chloro-5-methyl-(1,2,4)triazolo(1,5-a)pyrimidine-2-carboxylate

Product 1

HCID 178429722HCID 178429722, compoundYield 63.4%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
60 °C

Procedure

The product obtained in Step 1 (17 g) was added at a time, in a nitrogen atmosphere, to a solution of sodium hydrosulfide (16 g) in 280 ml of water at room temperature with stirring, and the mixture was heated to 60° C. with stirring continued. The resultant yellow solution was cooled to room temperature, the insoluble matters were filtered off, the filtrate was acidified with concentrated hydrochloric acid to pH 2.0, and the crystals thus formed were collected by filtration and washed twice with 20 ml of water, affording 10 g of the objective compound as yellow crystals.

Workup

  1. stirringwith stirring
  2. temperatureThe resultant yellow solution was cooled to room temperature
  3. filtrationthe insoluble matters were filtered off
  4. customthe crystals thus formed
  5. filtrationwere collected by filtration
  6. washwashed twice with 20 ml of water

Sources & evidence

ORD record
ord-303a68d156eb4db1aafd0c897715ff15
Source dataset
uspto-grants-1991_11
Patent number
US05064953

Reaction notes

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