1-Methylpiperazine → HCID 12902435, compound

HRID 1744505Notes

Reaction equation

HRID 1744505 reaction equation
Cl[C:2]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[CH:6][C:3]=1[C:4]#[N:5].C[N:14]1[CH2:19][CH2:18]N[CH2:16][CH2:15]1>C(O)C>[N+:10]([C:7]1[CH:8]=[CH:9][C:2]([N:14]([CH2:19][CH3:18])[CH2:15][CH3:16])=[C:3]([CH:6]=1)[C:4]#[N:5])([O-:12])=[O:11]

Participants

4

Reactant 2

HCID 531671-MethylpiperazineHCID 855042-Chloro-5-nitrobenzonitrile

Product 1

HCID 12902435HCID 12902435, compoundYield 70.5%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

2-Chloro-5-nitrobenzonitrile (15 g) and methylpiperazine (9.8 g) were added to ethanol (100 ml) and the mixture was stirred at a refluxing temperature for 1 h. The solvent was evaporated under reduced pressure. Diisopropyl ether was added to the residue to allow crystallization. The crystals were recrystallized from hydrous ethanol to give 5-nitro-2-diethylaminobenzonitrile (12.7 g), melting point: 83–85° C.

Workup

  1. customThe solvent was evaporated under reduced pressure
  2. additionDiisopropyl ether was added to the residue
  3. customcrystallization
  4. customThe crystals were recrystallized from hydrous ethanol

Sources & evidence

ORD record
ord-d337ecba074040888acdd9441f1562c6
Source dataset
uspto-grants-2006_03
Patent number
US07015218B1

Reaction notes

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