Hydrazine hydrate (1:1) → HCID 54026278, compound

HRID 224795Notes

Reaction equation

HRID 224795 reaction equation
C(O[C:4]([C:6]1[C:11](=[O:12])[N:10]2[CH:13]([CH3:25])[CH2:14][CH2:15][C:16](=[N:17][NH:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[C:9]2=[N:8][CH:7]=1)=[O:5])C.O.[NH2:27][NH2:28]>C(O)C>[C:19]1([NH:18][N:17]=[C:16]2[C:9]3=[N:8][CH:7]=[C:6]([C:4]([NH:27][NH2:28])=[O:5])[C:11](=[O:12])[N:10]3[CH:13]([CH3:25])[CH2:14][CH2:15]2)[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 53789031Ethyl 6,7,8,9-tetrahydro-6-methyl-4-oxo-9-(2-phenylhydrazinylidene)-4H-pyrido[1,2-a]pyrimidine-3-carboxylate

Product 1

HCID 54026278HCID 54026278, compoundYield 82.7%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

7.8 g. (0.02 mole) of ethyl-9-(phenyl-hydrazono)-6-methyl-4-oxo-6,7,8,9-tetrahydro-4H-pyrido(1,2-a)pyrimidine-3-carboxylate are dissolved in 100 ml. of ethanol. To the solution 6.0 ml. of 98% hydrazine-hydrate are added and the reaction mixture is refluxed for 2 hours. On cooling the precipitation of crystals begins. The crystals are filtered off and washed with ethanol. Thus 5.4 g. (82.7%) of 9-(phenyl-hydrazono)-6-methyl-4-oxo-6,7,8,9-tetrahydro-4H-pyrido(1,2-a)pyrimidine-3-carbohydrazide are obtained.

Workup

  1. temperaturethe reaction mixture is refluxed for 2 hours
  2. temperatureOn cooling
  3. customthe precipitation of crystals
  4. filtrationThe crystals are filtered off
  5. washwashed with ethanol

Sources & evidence

ORD record
ord-806ae1ff14f2448295318c3aeb03b22f
Source dataset
uspto-grants-1980_11
Patent number
US04234586

Reaction notes

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