Hydrazine hydrate (1:1) → HCID 21455999, compound

HRID 435598Notes

Reaction equation

HRID 435598 reaction equation
[N+:1]([C:4]1[N:8]([CH2:9][CH3:10])[C:7]([C:11]2[N:15]3[N:16]=[C:17](Cl)[CH:18]=[CH:19][C:14]3=[N:13][N:12]=2)=[N:6][CH:5]=1)([O-:3])=[O:2].O1CCOCC1.O.[NH2:28][NH2:29]>CO>[N+:1]([C:4]1[N:8]([CH2:9][CH3:10])[C:7]([C:11]2[N:15]3[N:16]=[C:17]([NH:28][NH2:29])[CH:18]=[CH:19][C:14]3=[N:13][N:12]=2)=[N:6][CH:5]=1)([O-:3])=[O:2]

Participants

5

Reactant 3

HCID 24654Hydrazine hydrate (1:1)HCID 312751,4-DioxaneHCID 21455976HCID 21455976, compound

Product 1

HCID 21455999HCID 21455999, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

3 g. 3-(5-nitro-1-ethyl-2-imidazolyl)-6-chloro-s-triazolo[4,3-b]pyridazine were dissolved in 30 ml. of a mixture of dioxan and methanol (1:1) and 3 ml. hydrazine hydrate were added thereto at 20° - 25° C., while stirring. The reaction mixture was further stirred for 45 minutes and the separated crystals were filtered off with suction, washed with a mixture of dioxan and methanol (1:1) and dried in a vacuum at 120° C. There was thus obtained 0.66 g. of the desired 3-(5-nitro-1-ethyl-2-imidazolyl)-6-hydrazino-s-triazolo[4,3-b]pyridazine which melts, with foaming up, at 216° - 223° C.

Workup

  1. stirringThe reaction mixture was further stirred for 45 minutes
  2. filtrationthe separated crystals were filtered off with suction
  3. washwashed with a mixture of dioxan and methanol (1:1)
  4. customdried in a vacuum at 120° C
  5. customwith foaming up, at 216° - 223° C.

Sources & evidence

ORD record
ord-9d70cbcbd0ab49cc8fc27f8459fb9305
Source dataset
uspto-grants-1977_02
Patent number
US04006141

Reaction notes

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