Hydrazine hydrate (1:1) → HCID 57197527, compound

HRID 224796Notes

Reaction equation

HRID 224796 reaction equation
Br[CH:2]1[C:7]2=[N:8][CH:9]=[C:10]([C:13]([NH2:15])=[O:14])[C:11](=[O:12])[N:6]2[CH:5]([CH3:16])[CH2:4][CH2:3]1.O.[NH2:18][NH2:19]>CO>[N:18](=[C:2]1[C:7]2=[N:8][CH:9]=[C:10]([C:13]([NH2:15])=[O:14])[C:11](=[O:12])[N:6]2[CH:5]([CH3:16])[CH2:4][CH2:3]1)[NH2:19]

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 13467782HCID 13467782, compound

Product 1

HCID 57197527HCID 57197527, compoundYield 46.5%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent2×

Procedure

In 150 ml. of methanol 10.0 g. (34.95 millimoles) of 9-bromo-6-methyl-4-oxo-6,7,8,9-tetrahydro-4H-pyrido(1,2-a)pyrimidine-3-carboxamide are dissolved under heating. To the solution 20 ml. hydrazine hydrate are added dropwise under stirring carefully within 10 minutes. The reaction mixture is heated to boiling for 40 minutes whereupon the methanol is distilled off in vacuo. The crystals are filtered off, washed with water and crystallized from water. Thus 3.8 g. (46.5%) of 9-hydrazono-6-methyl-4-oxo-6,7,8,9-tetrahydro-4H-pyrido(1,2-a)pyrimidine-3-carboxamide are obtained. Mp.: 248°-250° C.

Workup

  1. temperatureunder heating
  2. temperatureThe reaction mixture is heated
  3. distillationis distilled off in vacuo
  4. filtrationThe crystals are filtered off
  5. washwashed with water
  6. customcrystallized from water

Sources & evidence

ORD record
ord-da1c53e256bb4852910daa400c24ff7d
Source dataset
uspto-grants-1980_11
Patent number
US04234586

Reaction notes

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