Hydrochloric Acid → HCID 178433785, compound

HRID 1445696Notes

Reaction equation

HRID 1445696 reaction equation
[NH2:1][C:2]1[C:3](Br)=[CH:4][C:5]([F:16])=[C:6]([N:8]2[C:12](=[O:13])[N:11]([CH3:14])[C:10]([CH3:15])=[N:9]2)[CH:7]=1.CCO[C:21]([S-:23])=[S:22].[K+].Cl>CN(C)C=O>[F:16][C:5]1[C:6]([N:8]2[C:12](=[O:13])[N:11]([CH3:14])[C:10]([CH3:15])=[N:9]2)=[CH:7][C:2]2[N:1]=[C:21]([SH:23])[S:22][C:3]=2[CH:4]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 2735045Potassium ethylxanthateHCID 14625179HCID 14625179, compound

Product 1

HCID 178433785HCID 178433785, compoundYield 75%

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Conditions

Temperature
140 °C

Procedure

30 mL N,N-dimethylformamide was charged with 0.01 mol 1-(5-amino-4-bromo-2-fluorophenyl)-3,4-dimethyl-1H-1,2,4-triazol-5(4H)-one. The mixture was stirred until it became clear. 0.02 mol potassium ethyl xanthogenate was added to the mixture in two portions. The mixture was refluxed at 140° C. for 6 h, cooled, and poured into 100 mL ice water slurry. The mixture was acidified with 6 mol/L hydrochloric acid, and a large amount of solid materials crushed out. The title compound was obtained in a 75% yield as a white solid after filtration.

Workup

  1. temperaturecooled
  2. customa large amount of solid materials crushed out

Sources & evidence

ORD record
ord-2b50e17f21d94d01b13bfd3e455e309e
Source dataset
uspto-grants-2010_02
Patent number
US07666890B2

Reaction notes

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