反応式
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)CC1参加物
6
反応物 2
生成物 1
試薬・触媒・溶媒 3
反応条件
- 温度
- 160 °C
実験手順
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.
出典と根拠
- ORDレコード
- ord-c35b162a34bf408282b33e4af9af7634
- 出典データセット
- 750 AstraZeneca ELN dataset
- 元リンク
- 出典を表示
関連ノート
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