Formic Acid → HCID 19766996, compound

HRID 1197213Notes

Reaction equation

HRID 1197213 reaction equation
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([OH:11])(=[O:10])=[O:9])=[C:4]([NH2:12])[CH:3]=1.[OH-].[Na+].[C:15](OC(=O)C)(=[O:17])[CH3:16].Cl.[Cl-].[Na+].[CH:25](O)=[O:26]>O>[C:15]([NH:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([OH:11])(=[O:9])=[O:10])=[C:4]([NH:12][CH:25]=[O:26])[CH:3]=1)(=[O:17])[CH3:16]

Participants

8

Reactant 6

HCID 284Formic AcidHCID 313Hydrochloric AcidHCID 5234Sodium ChlorideHCID 7918Acetic AnhydrideHCID 14798Sodium Hydroxide2×HCID 666232,4-Diaminobenzenesulfonic acid

Product 1

HCID 19766996HCID 19766996, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

47 g of 1,3-diaminobenzene-4-sulfonic acid in 215 ml of water and 35 g of formic acid were heated under reflux for 3 hours. The pH was then adjusted to 6.5 with caustic soda solution and, at 20° C., 35 g of acetic anhydride were added dropwise, while the pH was kept between 6.0 and 7.0 with caustic soda solution. After 1 hour, the pH was adjusted to 4.0 with hydrochloric acid, and 200 g of sodium chloride were added. Stirring was continued for 5 hours, after which the precipitated 1-(N-acetylamino)-3-(N-formylamino)benzene-4-sulfonic acid was isolated by filtration.

Workup

  1. temperatureunder reflux for 3 hours
  2. additionwere added
  3. waitwas continued for 5 hours

Sources & evidence

ORD record
ord-dfaaa590fe69453ba3c189e0cc1543b2
Source dataset
uspto-grants-1992_05
Patent number
US05117050

Reaction notes

Loading…