Ethyl Acetoacetate → HCID 178429264, compound

HRID 27899Notes

Reaction equation

HRID 27899 reaction equation
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[N:8]=[N:9][C:10]([NH:13][NH2:14])=[CH:11][CH:12]=2)[CH2:3][CH2:2]1.[C:15](OCC)(=[O:20])[CH2:16][C:17]([CH3:19])=O.[OH-].[NH4+]>C(O)C>[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[N:8]=[N:9][C:10]([N:13]3[C:15]([OH:20])=[CH:16][C:17]([CH3:19])=[N:14]3)=[CH:11][CH:12]=2)[CH2:3][CH2:2]1

Participants

5

Reactant 3

HCID 8868Ethyl AcetoacetateHCID 14923Ammonium HydroxideHCID 12603548HCID 12603548, compound

Product 1

HCID 178429264HCID 178429264, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A mixture of 0.98 g (5 mmoles) of 3-morpholino-6-pyridazinyl-hydrazine, 0.65 g (5 mmoles) of ethyl acetoacetate and 15 ml of ethanol is stirred at reflux temperature for 3 hours. After cooling the mixture is stirred with 1 ml of concentrated aqueous ammonium hydroxide solution at room temperature for 4 hours and then left to stand overnight. The separated crystals are filtered, washed with water and recrystallized from ethanol. Yield: 0.5 g (39%); m.p.: 189°-192° C.

Workup

  1. temperatureat reflux temperature for 3 hours
  2. temperatureAfter cooling the mixture
  3. waitleft
  4. filtrationThe separated crystals are filtered
  5. washwashed with water
  6. customrecrystallized from ethanol

Sources & evidence

ORD record
ord-f214f96a84e4413894227dd708debb19
Source dataset
uspto-grants-1980_09
Patent number
US04224325

Reaction notes

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