Reaktion #1462178

Reaktionsgleichung

(2R)-4-benzyl-1-[3,5-bis(trifluoromethyl)-benzoyl]-2-(4-chloro-3-methoxybenzyl)piperazine

1-chloroethyl chloroformate

→

(2R)-1-[3,5-bis(trifluoromethyl)benzoyl]-2-(4-chloro-3-methoxybenzyl)piperazine hydrochloride

Ausbeute 198.0%

Lösungsmittel

1,2-dichloroethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder reflux for 15 hours
2. 2
   TemperaturAfter cooling
3. 3
   Einengenthe reaction mixture was concentrated under reduced pressure
4. 4
   workup.DISSOLUTIONThe resulting syrup was dissolved into methanol (10 ml)
5. 5
   Temperaturunder reflux for 2 hours
6. 6
   TemperaturAfter cooling
7. 7
   Einengenthe reaction mixture was concentrated under reduced pressure
8. 8
   Filtrationthe resulting powder was collected by filtration

Vorschrift

A solution of (2R)-4-benzyl-1-[3,5-bis(trifluoromethyl)-benzoyl]-2-(4-chloro-3-methoxybenzyl)piperazine (2.23 g) and 1-chloroethyl chloroformate (0.61 ml) in 1,2-dichloroethane (10 ml) was stirred under reflux for 15 hours. After cooling, the reaction mixture was concentrated under reduced pressure. The resulting syrup was dissolved into methanol (10 ml) and the solution was stirred under reflux for 2 hours. After cooling, the reaction mixture was concentrated under reduced pressure and the resulting powder was collected by filtration to give a yellow powder of (2R)-1-[3,5-bis(trifluoromethyl)benzoyl]-2-(4-chloro-3-methoxybenzyl)piperazine hydrochloride (2.00 g).

Quelle