1-Methylpiperazine → 2-Amino-6-(4-methyl-1-piperazinyl)-3-(2,3,5-trichlorophenyl)pyrazine

HRID 1358976Notes

Reaction equation

HRID 1358976 reaction equation
[NH2:1][C:2]1[C:7]([C:8]2[CH:13]=[C:12]([Cl:14])[CH:11]=[C:10]([Cl:15])[C:9]=2[Cl:16])=[N:6][CH:5]=[C:4](Cl)[N:3]=1.[CH3:18][N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1>>[NH2:1][C:2]1[C:7]([C:8]2[CH:13]=[C:12]([Cl:14])[CH:11]=[C:10]([Cl:15])[C:9]=2[Cl:16])=[N:6][CH:5]=[C:4]([N:22]2[CH2:23][CH2:24][N:19]([CH3:18])[CH2:20][CH2:21]2)[N:3]=1

Participants

3

Procedure

2-Amino-6-chloro-3-(2,3,5-trichlorophenyl)pyrazine (0.215 g, 7.0×10−3 mole) Example 1 Route A and 1-methylpiperazine (5 ml, Aldrich), were heated at 140° C. for 1 hr. The mixture was evaporated in vacuo and the residue was purified by ‘flash chromatography’ eluting with ethanol:dichloromethane, 0-4%. The product was dissolved in the minimum of dichloromethane and hexane (10 ml), added slowly to give yellow needles. Yield 0.247 g (95%), M.p. 185° C.

Workup

  1. customThe mixture was evaporated in vacuo
  2. customthe residue was purified by ‘flash chromatography’
  3. washeluting with ethanol
  4. dissolutionThe product was dissolved in the minimum of dichloromethane and hexane (10 ml)
  5. additionadded slowly
  6. customto give yellow needles

Sources & evidence

ORD record
ord-4dd537b53bf34caa8c39163707c8e6f5
Source dataset
uspto-grants-2003_07
Patent number
US06599905B2

Reaction notes

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