Reaktion #73795

Reaktionsgleichung

Aluminium chloride

1-(4-Bromo-phenyl)-2-methylamino-ethanol

Water

→

desired product

[2-(4-Bromo-phenyl)-2-(4-chloro-phenyl)-ethyl]-methyl-amine

Lösungsmittel

chlorobenzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe reaction mixture was then partitioned between dichloromethane (100 ml) and saturated NaHCO3 (30 ml)
2. 2
   TrocknenThe organic layer was dried (MgSO4)
3. 3
   Filtrationfiltered
4. 4
   Einengenconcentrated under reduced pressure
5. 5
   SonstigeThe crude product was then purified by Phenomenex_Strata_SCX column chromatography
6. 6
   Wascheneluting with methanol

Vorschrift

Aluminium chloride (278 mg, 2.087 mmol) was added portionwise to a stirred solution of 1-(4-Bromo-phenyl)-2-methylamino-ethanol (160 mg, 0.696 mmol) in chlorobenzene (3 ml) and the reaction mixture stirred at room temperature for 17 hours. Water (2 ml) was added dropwise and the reaction mixture was then partitioned between dichloromethane (100 ml) and saturated NaHCO3 (30 ml). The organic layer was dried (MgSO4), filtered and concentrated under reduced pressure. The crude product was then purified by Phenomenex_Strata_SCX column chromatography eluting with methanol followed by 2N ammonia in methanol to afford the desired product. LC/MS: (PS-B3) Rt 3.58 [M+H]+ 324.

Quelle