Carbon Disulfide → HCID 178506204, compound

HRID 476903Notes

Reaction equation

HRID 476903 reaction equation
[C:1](=[S:3])=S.[F:4][C:5]([F:15])([F:14])[C:6]1[C:7]([NH:12][NH2:13])=[N:8][CH:9]=[CH:10][CH:11]=1>N1C=CC=CC=1>[SH:3][C:1]1[N:8]2[CH:9]=[CH:10][CH:11]=[C:6]([C:5]([F:15])([F:14])[F:4])[C:7]2=[N:12][N:13]=1

Participants

4

Reactant 2

HCID 6348Carbon DisulfideHCID 27777762-Hydrazinyl-3-(trifluoromethyl)pyridine

Product 1

HCID 178506204HCID 178506204, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

16 ml of carbon disulfide are added dropwise at room temperature, with stirring, to a suspension of 40 g of 3-trifluoromethyl-2-hydrazinopyridine, prepared in Example 12, in 75 ml of pyridine. When the additioon is complete, stirring is continued for 15 minutes at room temperature and the reaction mixture is then heated under reflux for 5 hours. After cooling, the medium is concentrated in vacuo and water is then added. The solid residue obtained is filtered off, washed with water and dried to give 40 g of 3-mercapto-8-trifluoromethyl-1,2,4-triazolo(4,3-a)pyridine in the form of crystals melting at 236° C.

Workup

  1. temperaturethe reaction mixture is then heated
  2. temperatureunder reflux for 5 hours
  3. temperatureAfter cooling
  4. concentrationthe medium is concentrated in vacuo and water
  5. additionis then added
  6. customThe solid residue obtained
  7. filtrationis filtered off
  8. washwashed with water
  9. customdried

Sources & evidence

ORD record
ord-a55edcc8dff24222a6a3944319a25426
Source dataset
uspto-grants-1989_12
Patent number
US04886805

Reaction notes

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