1-Methylpiperazine → HCID 12781932, compound

HRID 918075Notes

Reaction equation

HRID 918075 reaction equation
Br[CH2:2][C:3]1[S:7][C:6]([C:8]2[O:9][C:10]3[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[CH:13][C:11]=3[N:12]=2)=[CH:5][CH:4]=1.[CH3:20][N:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1>C1C=CC=CC=1>[CH3:20][N:21]1[CH2:26][CH2:25][N:24]([CH2:2][C:3]2[S:7][C:6]([C:8]3[O:9][C:10]4[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[CH:13][C:11]=4[N:12]=3)=[CH:5][CH:4]=2)[CH2:23][CH2:22]1

Participants

4

Reactant 2

HCID 531671-MethylpiperazineHCID 12781927HCID 12781927, compound

Product 1

HCID 12781932HCID 12781932, compoundYield 73.9%

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Procedure

2-[5-(Bromomethyl)-2-thienyl]-5-nitrobenzoxazole (1.16 g, 0.0034 mole, prepared as described in Example 1) and N-methylpiperazine (1.4 g, 0.014 mole) are dissolved in 50 ml of benzene and heated at reflux for 24 hours. The precipitated N-methylpiperazine hydrobromide is removed by filtration and the benzene removed under vacuum yielding a solid. Crystallization from ethanol yields 0.9 g of the title compound, melting point 135°-137°C.

Workup

  1. temperatureheated
  2. temperatureat reflux for 24 hours
  3. customThe precipitated N-methylpiperazine hydrobromide is removed by filtration
  4. customthe benzene removed under vacuum
  5. customyielding a solid
  6. customCrystallization from ethanol

Sources & evidence

ORD record
ord-0171cdeb080348eea407adcce92dae27
Source dataset
uspto-grants-1976_07
Patent number
US03969351

Reaction notes

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