Hydrochloric Acid → HCID 178429343, compound

HRID 2387746Notes

Reaction equation

HRID 2387746 reaction equation
[Na].[C:2]([O:8]CC)(=O)[CH2:3][C:4]([CH3:6])=O.Cl.[C:12]([NH2:15])(=[NH:14])[CH3:13].Cl>C(O)C>[CH3:13][C:12]1[N:15]=[C:2]([OH:8])[CH:3]=[C:4]([CH3:6])[N:14]=1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 8868Ethyl AcetoacetateHCID 67170Acetamidine monohydrochlorideHCID 5360545Sodium

Product 1

HCID 178429343HCID 178429343, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Sodium (3.6 g) was added by portions to ethanol (92 ml) over 2 hours, while the solution was stirred at room temperature. Thereafter, ethyl acetoacetate (10 ml) and acetamidine hydrochloride (7.42 g) were added to the reaction solution, and the obtained mixture was stirred at 70° C. for 16 hours. Thereafter, the reaction mixture was stirred at 100° C. for 9 hours, and the temperature of the reaction solution was returned to room temperature. Concentrated hydrochloric acid was added to the reaction solution, so that the pH value was adjusted to around 5. The obtained mixture was concentrated under reduced pressure, so as to obtain a crude title compound (25.6 g).

Workup

  1. stirringthe obtained mixture was stirred at 70° C. for 16 hours
  2. stirringThereafter, the reaction mixture was stirred at 100° C. for 9 hours
  3. customwas returned to room temperature
  4. concentrationThe obtained mixture was concentrated under reduced pressure

Sources & evidence

ORD record
ord-93b100087fdc40fb853b882ce6f8d1c3
Source dataset
uspto-grants-2012_09
Patent number
US08268848B2

Reaction notes

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