3-Chloro-2-methylaniline → 1-(3-Chloro-2-methylphenyl)piperazine

HRID 339733

Reaktionsgleichung

Reaktionsgleichung von HRID 339733
[Cl:1][C:2]1[C:3]([CH3:9])=[C:4]([CH:6]=[CH:7][CH:8]=1)[NH2:5].Cl.Cl[CH2:12][CH2:13][NH:14][CH2:15][CH2:16]Cl.C([O-])([O-])=O.[Na+].[Na+]>C(O)CCC>[Cl:1][C:2]1[C:3]([CH3:9])=[C:4]([N:5]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)[CH:6]=[CH:7][CH:8]=1

Komponenten

5

Edukt 3

HCID 68943-Chloro-2-methylanilineHCID 10340Sodium CarbonateHCID 522769Bis(2-chloroethyl)amine hydrochloride

Produkt 1

HCID 38008451-(3-Chloro-2-methylphenyl)piperazineAusbeute 81 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 2631-ButanolLösungsmittel

Versuchsvorschrift

To a stirred solution of 3-chloro-2-methylaniline (21.6 g, 0.15 mol) in n-butanol (200 ml) was added bis(2-chloroethyl)amine hydrochloride (30 g, 0.17 mol) at room temperature and allowed to refluxed temperature for 2 days. After cooled to room temperature Na2CO3 (9 g, 0.08 mol) was added and then reaction mixture was refluxed 30 min. The resulting mixture was filtered with n-butanol (100 ml) and collected solid was dried under reduced pressure to be obtained title compound (24.8 g, 81%) as white solid.

Aufarbeitung

  1. temperatureto refluxed temperature for 2 days
  2. additionwas added
  3. customreaction mixture
  4. temperaturewas refluxed 30 min
  5. filtrationThe resulting mixture was filtered with n-butanol (100 ml)
  6. customcollected solid
  7. customwas dried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-1cf06a9b55ae4c158ce1dc46b354b071
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08895558B2

Verknüpfte Notizen

Wird geladen…