Acetonitrile → HCID 135735631, compound

HRID 127340Notes

Reaction equation

HRID 127340 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])=[CH:23][C:22]=2[CH3:32])[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])=[CH:23][C:22]=2[CH3:32])[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 135735633HCID 135735633, compound

Product 1

HCID 135735631HCID 135735631, compound

Reagents, catalysts & solvents 1

HCID 31374DimethylacetamideSolvent

Procedure

To a solution containing 25 g of the naphthol compound obtained in Step (1) above, 180 ml of acetonitrile and 35 ml of phosphorus oxychloride, 15 ml of N,N-dimethylacetamide was added dropwise at a temmperature below 60° C. with stirring. The mixture was stirred at 60° C. for 3 hours and was poured into 800 ml 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 temmperature 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-ac8696cc5ae747abb676b51578c434a6
Source dataset
uspto-grants-1981_03
Patent number
US04255509

Reaction notes

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