Hydrochloric Acid → HCID 178469410, compound

HRID 477547Notes

Reaction equation

HRID 477547 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 at a time 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-4a3fff3814b74982a29a10e3e401dc5b
Source dataset
uspto-grants-1989_12
Patent number
US04888332

Reaction notes

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