1-Methylpiperazine → HCID 21537484, compound

HRID 1076662Notes

Reaction equation

HRID 1076662 reaction equation
[N+:1]([C:4]1[O:8][C:7]([C:9]2[N:13]3[N:14]=[C:15]([N:18]=[CH:19]OCC)[CH:16]=[CH:17][C:12]3=[N:11][N:10]=2)=[CH:6][CH:5]=1)([O-:3])=[O:2].[CH3:23][N:24]1[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]1>O1CCOCC1>[N+:1]([C:4]1[O:8][C:7]([C:9]2[N:13]3[N:14]=[C:15]([N:18]=[CH:19][N:27]4[CH2:28][CH2:29][N:24]([CH3:23])[CH2:25][CH2:26]4)[CH:16]=[CH:17][C:12]3=[N:11][N:10]=2)=[CH:6][CH:5]=1)([O-:3])=[O:2]

Participants

4

Reactant 2

HCID 531671-MethylpiperazineHCID 21537501HCID 21537501, compound

Product 1

HCID 21537484HCID 21537484, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

0.9 g. 3-(5-nitro-2-furyl)-6-(ethyoxymethyleneamino)-s-triazolo[4,3-b]pyridazine were dissolved in 20 ml. hot dioxan and mixed, while stirring, with 0.6 g. N-methyl-piperazine at 50°C. After 15 minutes, the crystals formed were filtered off with suction and recrystallized from 15 ml. of a mixture of 70% dioxan and 30 ml. dimethyl formamide. There was thus obtained 0.77 g. 3-(5-nitro-2-furyl)-6-(4-methyl-1-piperazinyl methyleneamino)-s-triazolo[4,3-b]pyridazine, which had a melting point of 247° - 248°C.

Workup

  1. customat 50°C
  2. customthe crystals formed
  3. filtrationwere filtered off with suction
  4. customrecrystallized from 15 ml
  5. additionof a mixture of 70% dioxan and 30 ml

Sources & evidence

ORD record
ord-d8612fddc0874980bc8936c480358665
Source dataset
uspto-grants-1976_05
Patent number
US03957766

Reaction notes

Loading…