Reaktion #66529

Reaktionsgleichung

Picolinoyl chloride hydrochloride

Et3N

tert-butyl 4-(4-amino-2-chlorophenyl)piperazine-1-carboxylate

→

tert-butyl 4-(2-chloro-4-(picolinamido)phenyl)piperazine-1-carboxylate

Ausbeute 100.0%

Lösungsmittel

DCM

Reaktionsbedingungen

Aufarbeitung

1. 1
   WaschenThe organic phase was washed with a saturated solution of NaHCO3
2. 2
   ExtraktionThe aqueous phase was extracted with AcOEt
3. 3
   WaschenThe organic phase was washed with brine
4. 4
   Trocknenwas dried over Na2SO4
5. 5
   Filtrationwas filtered
6. 6
   Einengenwas concentrated under reduced pressure

Vorschrift

According to Scheme 5 Step 3: Picolinoyl chloride hydrochloride (3.68 mmol, 656 mg) and Et3N (7.37 mmol, 1.03 mL) were added to a solution of tert-butyl 4-(4-amino-2-chlorophenyl)piperazine-1-carboxylate (2.46 mmol, 766 mg) in DCM (40 mL) at 0° C. The reaction mixture was stirred at room temperature for 1 hour. The organic phase was washed with a saturated solution of NaHCO3. The aqueous phase was extracted with AcOEt. The organic phase was washed with brine, was dried over Na2SO4, was filtered and was concentrated under reduced pressure to afford tert-butyl 4-(2-chloro-4-(picolinamido)phenyl)piperazine-1-carboxylate (2.46 mmol, 1.02 g, 100%).

Quelle