Methane → HCID 21455932, compound

HRID 1729872Notes

Reaction equation

HRID 1729872 reaction equation
[N+:1]([C:4]1[N:8]([CH2:9][CH2:10][O:11]C(=O)C)[C:7]([C:15]2[N:19]3[N:20]=[C:21]([N:24]4[CH2:29][CH2:28][N:27]([CH3:30])[CH2:26][CH2:25]4)[CH:22]=[CH:23][C:18]3=[N:17][N:16]=2)=[N:6][CH:5]=1)([O-:3])=[O:2].Cl.C>>[N+:1]([C:4]1[N:8]([CH2:9][CH2:10][OH:11])[C:7]([C:15]2[N:19]3[N:20]=[C:21]([N:24]4[CH2:25][CH2:26][N:27]([CH3:30])[CH2:28][CH2:29]4)[CH:22]=[CH:23][C:18]3=[N:17][N:16]=2)=[N:6][CH:5]=1)([O-:3])=[O:2]

Participants

4

Reactant 3

HCID 297MethaneHCID 313Hydrochloric AcidHCID 21455926HCID 21455926, compound

Product 1

HCID 21455932HCID 21455932, compound

Procedure

1.8 g. 3-(5-nitro- 1-β-acetoxyethyl-2-imidazolyl)-6-(4-methyl-1-piperazinyl)-s-triazolo[4,3-b]pyridazine (obtained according to Example 23) was reacted for 1.5 hours at 50° C. with 36 ml. 2N hydrochloric acid. The solution was then treated with charcoal, evaporated in a vacuum and the residue dissolved in 10 ml. water, adjusted to about pH 9 with concentrated aqueous ammonia, left to stand for about 30 minutes and the precipitated crystals were filtered off with suction and washed with water and ether. There was thus obtained 1.1 g. of the desired 3-(5-nitro-1-β-hydroxyethyl-2-imidazolyl)-6-(4-methyl-1-piperazinyl)-s-triazolo[4,3-b]pyridazine. After drying for 1.5 days in a vacuum at 70° C., the product has a melting point of 98° - 100° C. (foams up).

Workup

  1. customevaporated in a vacuum
  2. dissolutionthe residue dissolved in 10 ml
  3. waitleft
  4. filtrationthe precipitated crystals were filtered off with suction
  5. washwashed with water and ether
  6. customAfter drying for 1.5 days in a vacuum at 70° C.

Sources & evidence

ORD record
ord-5992114c520d414f95ecab076f45aef0
Source dataset
uspto-grants-1976_11
Patent number
US03989832

Reaction notes

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