Acetonitrile → HCID 135735630, compound

HRID 127341Notes

Reaction equation

HRID 127341 reaction equation
[C:1]([NH:5][S:6]([C:9]1[CH:18]=[C:17]([N:19]=[N:20][C:21]2[CH:26]=[C:25]([CH3:27])[C:24]([S:28](O)(=[O:30])=[O:29])=[C:23]([CH3:32])[CH:22]=2)[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][C:15]=2[NH:33][S:34]([CH3:37])(=[O:36])=[O:35])[C:10]=1[OH:38])(=[O:8])=[O:7])([CH3:4])([CH3:3])[CH3:2].C(#N)C.P(Cl)(Cl)([Cl:44])=O>CN(C)C(=O)C>[C:1]([NH:5][S:6]([C:9]1[CH:18]=[C:17]([N:19]=[N:20][C:21]2[CH:26]=[C:25]([CH3:27])[C:24]([S:28]([Cl:44])(=[O:30])=[O:29])=[C:23]([CH3:32])[CH:22]=2)[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][C:15]=2[NH:33][S:34]([CH3:37])(=[O:36])=[O:35])[C:10]=1[OH:38])(=[O:8])=[O:7])([CH3:4])([CH3:3])[CH3:2]

Participants

5

Reactant 3

HCID 6342AcetonitrileHCID 24813Phosphorus oxychlorideHCID 1357356362-(N-tert-butylsulfamoyl)-4-(3,5-dimethyl-4-sulfophenylazo)-5-methanesulfonamido-1-naphthol

Product 1

HCID 135735630HCID 135735630, compound

Reagents, catalysts & solvents 1

HCID 31374DimethylacetamideSolvent

Procedure

To a solution containing 30 g of the naphthol compound obtained in Step (1) above, 250 ml to acetonitrile and 45 ml of phosphorus oxychloride, 15 ml of N,N-dimethylacetamide was added dropwise at a temperature below 60° C. with stirring. The mixture was stirred at 60° C. for 3 hours and poured into 1 l of ice water. The cyrstals thus-precipitated were collected by filtration and washed with 100 ml of acetonitrile.

Workup

  1. additionwas added dropwise at a temperature below 60° C.
  2. stirringThe mixture was stirred at 60° C. for 3 hours
  3. customThe cyrstals thus-precipitated
  4. filtrationwere collected by filtration
  5. washwashed with 100 ml of acetonitrile

Sources & evidence

ORD record
ord-b9eea556b325483d86161aa6132ac222
Source dataset
uspto-grants-1981_03
Patent number
US04255509

Reaction notes

Loading…