Ethyl Acetoacetate → HCID 178488949, compound

HRID 1082082

Reaction equation

HRID 1082082 reaction equation
Cl.[CH3:2][O:3][C:4]1[CH:12]=[CH:11][C:7]([C:8]([NH2:10])=[NH:9])=[CH:6][CH:5]=1.[C:13](OCC)(=[O:18])[CH2:14][C:15]([CH3:17])=O.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[OH:18][C:13]1[CH:14]=[C:15]([CH3:17])[N:10]=[C:8]([C:7]2[CH:11]=[CH:12][C:4]([O:3][CH3:2])=[CH:5][CH:6]=2)[N:9]=1

Participants

5

Reactant 3

HCID 8868Ethyl AcetoacetateHCID 11430Potassium CarbonateHCID 123262194-Methoxybenzamidine Hydrochloride

Product 1

HCID 178488949HCID 178488949, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To the mixture of 10 g of 4-methoxybenzamidine hydrochloride, 7.7 g of ethyl acetoacetate and 16.3 g of potassium carbonate were added 120 ml of ethanol, and the mixture was heat-refluxed with stirring for 7 hours. The reaction mixture was cooled and filtered to remove insoluble substances. The filtrate was evaporated. Water was added to the residue to dissolve and then the resulting solution was neutralized with acetic acid. The precipitated crystals were filtered off, washed with water and dried. Whereby 10.9 g of the desired substance was obtained as white crystals. Melting point is 202° to 203° C.

Workup

  1. temperaturethe mixture was heat-refluxed
  2. temperatureThe reaction mixture was cooled
  3. filtrationfiltered
  4. customto remove insoluble substances
  5. customThe filtrate was evaporated
  6. additionWater was added to the residue
  7. dissolutionto dissolve
  8. filtrationThe precipitated crystals were filtered off
  9. washwashed with water
  10. customdried
  11. customWhereby 10.9 g of the desired substance was obtained as white crystals

Sources & evidence

ORD record
ord-23fbbe22de624dc692ed81c6ea82baf6
Source dataset
uspto-grants-1996_12
Patent number
US05589477

Linked notes

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