1,4-Dibromobenzene → Methyl 1-(4-bromophenyl)pyrrolidine-3-carboxylate

HRID 519

Reaktionsgleichung

Reaktionsgleichung von HRID 519
Brc1ccc(Br)cc1.COC(=O)C1CCNC1>CC(C)(C)[O-].Cc1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.[Na+].[Pd].[Pd].c1ccc(P(c2ccccc2)c2ccc3ccccc3c2-c2c(P(c3ccccc3)c3ccccc3)ccc3ccccc23)cc1>COC(=O)C1CCN(c2ccc(Br)cc2)C1

Komponenten

7

Reaktionsbedingungen

Temperatur
85 °C

Versuchsvorschrift

A suspension of methyl pyrrolidine-3-carboxylate (800 mg, 6.19 mmol), 1,4-dibromobenzene (1461 mg, 6.19 mmol), TRIS(DIBENZYLIDENEACETONE)DIPALLADIUM(0) (142 mg, 0.15 mmol), 2,2'-bis(diphenylphosphino)-1,1'-binaphthyl (289 mg, 0.46 mmol) and Sodium Tert-Butoxide (714 mg, 7.43 mmol) in anhydrous toluene (30 mL) was stirred at 85 °C under nitrogen for 4 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 methyl 1-(4-bromophenyl)pyrrolidine-3-carboxylate (513 mg, 29.1 %) as a yellow solid.

Quellen und Nachweise

ORD-Eintrag
ord-cb0ae83e039e422babb6d81e64a4df69
Quelldatensatz
750 AstraZeneca ELN dataset
Originallink
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