2-Bromopyridine → (4-Cyclobutyl-piperazin-1-yl)-(6-pyridin-2-yl-6-aza-spiro[2.5]oct-1-yl)-methanone

HRID 732

Reaktionsgleichung

Reaktionsgleichung von HRID 732
Brc1ccccn1.O=C(C1CC12CCNCC2)N1CCN(C2CCC2)CC1>CC(=O)O.CC(=O)O.CC(C)(C)[O-].CC(C)c1cc(C(C)C)c(-c2ccccc2P(C2CCCCC2)C2CCCCC2)c(C(C)C)c1.[Na+].[Pd]>O=C(C1CC12CCN(c1ccccn1)CC2)N1CCN(C2CCC2)CC1

Komponenten

6

Reaktionsbedingungen

Temperatur
160 °C

Versuchsvorschrift

Reagents were put in a sealed vial and heated in the microwave oven for 10 minutes at 160°C. According to LC-MS analysis, the conversion is >90%. The crude mixture was transferred to a round-bottomed flask and volatiles were evaporated under vacuum. The residue was purified on preparative HPLC using the long high pH (acetonitrile in water ammonium carbonate buffer, 25 min.) 20 to 40% gradient method on XBridge Prep C18 OBD, 30x150 mm, 5 mm, Waters reverse phase column, giving (4-cyclobutylpiperazin-1-yl)(6-(pyridin-2-yl)-6-azaspiro[2.5]octan-1-yl)methanone (7.20 mg, 9.39 %). However, the compound was not pure enought for submission and there was not enough of it to attempt another purification.

Quellen und Nachweise

ORD-Eintrag
ord-c35b162a34bf408282b33e4af9af7634
Quelldatensatz
750 AstraZeneca ELN dataset
Originallink
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