Reaktion #828

ord-c35b162a34bf408282b33e4af9af7634

Reaktionsgleichung

Brc1ccccn1
Brc1ccccn1
O=C(C1CC12CCNCC2)N1CCN(C2CCC2)CC1
O=C(C1CC12CCNCC2)N1C
O=C(C1CC12CCN(c1ccccn1)CC2)N1CCN(C2CCC2)CC1
O=C(C1CC12CCN(c1cccc
Ausbeute 9.4%

Reaktionsbedingungen

Temperatur
160°CELSIUS

Vorschrift

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.

Quelle

750 AstraZeneca ELN dataset