Sodium hydrosulfide → HCID 178429722, compound

HRID 477516Notes

Reaction equation

HRID 477516 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. M.P.: 215.4°-217.3° C.

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-91d107bebee5465a8ff8a8adc8a73e64
Source dataset
uspto-grants-1989_12
Patent number
US04888332

Reaction notes

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