Potassium Acetate → HCID 21288295, compound

HRID 1249366Notes

Reaction equation

HRID 1249366 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-93c285f684d448758ddeee49c9ec9571
Source dataset
uspto-grants-1986_12
Patent number
US04631278

Reaction notes

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