Reaktion #614

ord-6d4c20d55c834a949848dd34c3fa431d

Reaktionsgleichung

Brc1ccc(Br)cc1
Brc1ccc(Br)cc1
CCOC(=O)C1CCNCC1
CCOC(=O)C1CCNCC1
CCOC(=O)C1CCN(c2ccc(Br)cc2)CC1
CCOC(=O)C1CCN(c2ccc(
Ausbeute 59.1%

Lösungsmittel

Reaktionsbedingungen

Temperatur
85°CELSIUS

Vorschrift

A suspension of ethyl piperidine-4-carboxylate (3.27 mL, 21.20 mmol), 1,4-dibromobenzene (5 g, 21.20 mmol), TRIS(DIBENZYLIDENEACETONE)DIPALLADIUM(0) (0.485 g, 0.53 mmol), 2,2'-bis(diphenylphosphino)-1,1'-binaphthyl (0.990 g, 1.59 mmol) and Sodium Tert-Butoxide (2.444 g, 25.43 mmol) in anhydrous toluene (60 mL) was stirred at 85 °C under nitrogen for 16 hours. The reaction was cooled to ambient temperature, diluted with Ether (100 mL) and filtered through celite. The filtrate was evaporated in vacuo to yield crude product. The crude product was purified by flash silica chromatography, elution gradient 0 to 20% EtOAc in heptane. Pure fractions were evaporated to dryness to afford ethyl 1-(4-bromophenyl)piperidine-4-carboxylate (3.91 g, 59.1 %) as a yellow oil.

Quelle

750 AstraZeneca ELN dataset