Hydrochloric Acid → HCID 178469410, compound

HRID 973852Notes

Reaction equation

HRID 973852 reaction equation
Cl[C:2]1[N:7]2[C:8]([CH3:11])=[N:9][N:10]=[C:6]2[N:5]=[C:4]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:3]=1.[SH-:17].[Na+].Cl>O>[CH2:15]([O:14][C:12]([C:4]1[CH:3]=[C:2]([SH:17])[N:7]2[C:8]([CH3:11])=[N:9][N:10]=[C:6]2[N:5]=1)=[O:13])[CH3:16]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 28015Sodium hydrosulfideHCID 148504555-Chloro-7-ethoxycarbonyl-3-methyl-s-triazolo[4,3-a]pyrimidine

Product 1

HCID 178469410HCID 178469410, compoundYield 80.8%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

The product obtained in Step 2 (4.0 g) was added all at once under ice cooling to a solution of 4.0 g of sodium hydrosulfide in 100 ml of water with stirring in nitrogen, and the mixture was stirred at room temperature overnight. The resulting solution was acidified to pH 1.0 with 6N hydrochloric acid, and the separated crystals were collected by filtration and recrystallized from ethanol, affording 3.2 g of the objective compound as orange crystals.

Workup

  1. stirringthe mixture was stirred at room temperature overnight
  2. filtrationthe separated crystals were collected by filtration
  3. customrecrystallized from ethanol

Sources & evidence

ORD record
ord-657ec52b6ea14fa9839339d538bcdc3c
Source dataset
uspto-grants-1991_11
Patent number
US05064953

Reaction notes

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