Potassium Carbonate → HCID 178488708, compound

HRID 1082084Notes

Reaction equation

HRID 1082084 reaction equation
Cl.[C:2]([NH2:5])(=[NH:4])[CH3:3].[CH3:6][O:7][C:8]1[CH:21]=[CH:20][C:11]([C:12]([CH2:14][C:15](OCC)=[O:16])=O)=[CH:10][CH:9]=1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[OH:16][C:15]1[CH:14]=[C:12]([C:11]2[CH:10]=[CH:9][C:8]([O:7][CH3:6])=[CH:21][CH:20]=2)[N:5]=[C:2]([CH3:3])[N:4]=1

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 67170Acetamidine monohydrochlorideHCID 76150Benzenepropanoic acid, 4-methoxy-beta-oxo-, ethyl ester

Product 1

HCID 178488708HCID 178488708, compoundYield 25.5%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

1.89 g of acetamidine hydrochloride and 4.44 g of etyl paramethoxybenzoylacetate were dissolved in 40 ml of ethanol. After addition of 5.52 g of potassium carbonate, the solution was refluxed with stirring for 8 hours, and then evaporated in vacuo. 5 g of sodium hydroxide was dissolved in 30 ml of water and this was added to the evaporated residue. Add ether, then extract, the aqueous layer was neutralized with acetic acid. The resulting precipitations were filtered off, washed with water and dried. Then 1.1 g of crystals were obtained. Melting point is 270° to 272° C.

Workup

  1. temperaturethe solution was refluxed
  2. customevaporated in vacuo
  3. dissolution5 g of sodium hydroxide was dissolved in 30 ml of water
  4. additionthis was added to the evaporated residue
  5. extractionAdd ether, then extract
  6. customThe resulting precipitations
  7. filtrationwere filtered off
  8. washwashed with water
  9. customdried

Sources & evidence

ORD record
ord-059d149148604995bdcb91bd237221cd
Source dataset
uspto-grants-1996_12
Patent number
US05589477

Reaction notes

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