1-Methylpiperazine → 1-Methyl-4-(5-nitro-2-pentafluoroethyl-benzyl)-piperazine

HRID 889953Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 889953
Br[CH2:2][C:3]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[CH:6]=[CH:5][C:4]=1[C:12]([F:18])([F:17])[C:13]([F:16])([F:15])[F:14].[CH3:19][N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1>>[CH3:19][N:20]1[CH2:25][CH2:24][N:23]([CH2:2][C:3]2[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[CH:6]=[CH:5][C:4]=2[C:12]([F:18])([F:17])[C:13]([F:16])([F:15])[F:14])[CH2:22][CH2:21]1

Komponenten

3

Edukt 2

HCID 531671-MethylpiperazineHCID 219593672-Bromomethyl-4-nitro-1-pentafluoroethyl-benzene

Produkt 1

HCID 222492671-Methyl-4-(5-nitro-2-pentafluoroethyl-benzyl)-piperazine

Versuchsvorschrift

2-Bromomethyl-4-nitro-1-pentafluoroethyl-benzene (2.6 g) was added to N-methylpiperazine (5 ml) and stirred at RT for 3 h. The mixture was filtered and the filtrate was treated with 1-chlorobutane, extracted with 2N HCl (100 ml). The acidic solution was treated with 5N NaOH (6 ml) then extracted with EtOAc. The organic layer was removed, dried over MgSO4 and concentrated to give the compound as an oil.

Aufarbeitung

  1. filtrationThe mixture was filtered
  2. additionthe filtrate was treated with 1-chlorobutane
  3. extractionextracted with 2N HCl (100 ml)
  4. additionThe acidic solution was treated with 5N NaOH (6 ml)
  5. extractionthen extracted with EtOAc
  6. customThe organic layer was removed
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-8142b73c9ec843119837bb0f9418562a
Quelldatensatz
uspto-grants-2006_02
Patentnummer
US06995162B2

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