Reaktion #616

ord-7673f35cb6ca4307811eaa7801ce679c

Reaktionsgleichung

Brc1ccc(Br)cc1
Brc1ccc(Br)cc1
COC(=O)C1CCNC1
COC(=O)C1CCNC1
COC(=O)C1CCN(c2ccc(Br)cc2)C1
COC(=O)C1CCN(c2ccc(B
Ausbeute 31.6%

Lösungsmittel

Reaktionsbedingungen

Temperatur
85°CELSIUS

Vorschrift

A suspension of methyl pyrrolidine-3-carboxylate (2.1 g, 16.26 mmol), 1,4-dibromobenzene (3.84 g, 16.26 mmol), TRIS(DIBENZYLIDENEACETONE)DIPALLADIUM(0) (0.372 g, 0.41 mmol), 2,2'-bis(diphenylphosphino)-1,1'-binaphthyl (0.759 g, 1.22 mmol) and Sodium Tert-Butoxide (1.875 g, 19.51 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 5 to 20% EtOAc in heptane. Pure fractions were evaporated to dryness to afford methyl 1-(4-bromophenyl)pyrrolidine-3-carboxylate (1.460 g, 31.6 %) as a yellow solid.

Quelle

750 AstraZeneca ELN dataset