HCID 10754419, compound → HCID 10777112, compound

HRID 2210449Notes

Reaction equation

HRID 2210449 reaction equation
[NH2:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[S:8]([NH:11][C:12](=O)[C:13]([F:16])([F:15])[F:14])(=[O:10])=[O:9]>P(Cl)(Cl)(Cl)=O>[F:14][C:13]([F:16])([F:15])[C:12]1[NH:1][C:2]2[CH:7]=[CH:6][N:5]=[CH:4][C:3]=2[S:8](=[O:10])(=[O:9])[N:11]=1

Participants

3

Reactant 1

HCID 10754419HCID 10754419, compound

Product 1

HCID 10777112HCID 10777112, compound

Reagents, catalysts & solvents 1

HCID 24813Phosphorus oxychlorideSolvent

Procedure

A mixture of 1 g of 4-amino-3-trifluoroacetylaminosulfonylpyridine (Preparation 18) and 20 cm3 of phosphorus oxychloride is brought to reflux for 18 hours. The solvent is removed under partial vacuum and the oil obtained, triturated with 5 ml of ice-cold water, produces a precipitate. The latter is collected on a filter, washed with water and dried. It is then purified by dissolving in the minimum amount of methanol and then adding 3 volumes of diethyl ether and 3 volumes of petroleum ether (40°-60° ). The crystals obtained are collected on a filter, washed with diethyl ether and dried.

Workup

  1. temperatureto reflux for 18 hours
  2. customThe solvent is removed under partial vacuum
  3. customthe oil obtained
  4. customtriturated with 5 ml of ice-cold water
  5. customproduces a precipitate
  6. customThe latter is collected on a filter
  7. washwashed with water
  8. customdried
  9. customIt is then purified
  10. dissolutionby dissolving in the minimum amount of methanol
  11. additionadding 3 volumes of diethyl ether and 3 volumes of petroleum ether (40°-60° )
  12. customThe crystals obtained
  13. customare collected on a filter
  14. washwashed with diethyl ether
  15. customdried

Sources & evidence

ORD record
ord-b347e476e4b143f48f953fa154bb28ea
Source dataset
uspto-grants-1995_10
Patent number
US05459138

Reaction notes

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