Potassium Acetate → HCID 21288295, compound

HRID 868308Notes

Reaction equation

HRID 868308 reaction equation
C([O:3][C:4](=O)[NH:5][C:6](=[O:28])[C:7]([C:26]#[N:27])=[N:8][NH:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]([C:24]#[N:25])([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH3:17])=[CH:12][CH:11]=1)C.C([O-])(=O)C.[K+]>C(O)(=O)C>[C:24]([C:16]([C:13]1[CH:14]=[CH:15][C:10]([N:9]2[C:4](=[O:3])[NH:5][C:6](=[O:28])[C:7]([C:26]#[N:27])=[N:8]2)=[CH:11][CH:12]=1)([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[CH3:17])#[N:25]

Participants

4

Reactant 2

HCID 517044Potassium AcetateHCID 131714994HCID 131714994, compound

Product 1

HCID 21288295HCID 21288295, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

A mixture of 7.8 parts of ethyl[2-cyano-2-[[4-(1-cyano-1-phenylethyl)phenyl]hydrazono]acetyl]carbamate, 1.98 parts of anhydrous potassium acetate and 120 parts of acetic acid was stirred and refluxed for 3 hours. The reaction mixture was concentrated to a volume of 30 parts. Water was added till the product was precipitated. It was sucked off, washed with water and dissolved in trichloromethane. The remaining water was separated and the organic phase was dried, filtered and evaporated, yielding 6.86 parts of 2-[4-(1-cyano-1-phenylethyl)phenyl]-2,3,4,5-tetrahydro-3,5-dioxo-1,2,4-triazine-6-carbonitrile as a residue (intermediate 65).

Workup

  1. temperaturerefluxed for 3 hours
  2. concentrationThe reaction mixture was concentrated to a volume of 30 parts
  3. additionWater was added till the product
  4. customwas precipitated
  5. washwashed with water
  6. dissolutiondissolved in trichloromethane
  7. customThe remaining water was separated
  8. customthe organic phase was dried
  9. filtrationfiltered
  10. customevaporated

Sources & evidence

ORD record
ord-fca25bdef7204f91b7e1b14b44191800
Source dataset
uspto-grants-1988_10
Patent number
US04778887

Reaction notes

Loading…