反応式
[CH3:1][O:2][CH:3](OC)[N:4]([CH3:6])C.[NH:9]1[CH2:13][CH2:12][CH2:11][CH2:10]1.[CH3:14]N(C)C=O>[Pd]>[CH3:1][O:2][C:3]1[CH:14]=[C:11]2[CH:12]=[CH:13][NH:9][C:10]2=[CH:6][N:4]=1参加物
5
反応条件
- 温度
- 100 °C
実験手順
10.76 g of N,N-dimethylformamide dimethyl acetal and 2.45 ml of pyrrolidine are added, in succession, to a solution of 5 g of the product obtained in Step 1 in 60 ml of dimethylformamide. The mixture obtained is first heated at 100° C. for 8 hours and then at 150° C. for 1 hour. Concentration is carried out under a vacuum of 10−1 mbar and the residue is taken up in 150 ml of tetrahydrofuran. The solution obtained is hydrogenated under a pressure of 10 bars for 4 hours in the presence of 10% Pd/C. After filtration and concentration, the residue is chromatographed over silica (eluant CH2Cl2/EtOH: 95/5) to yield the expected product.
後処理
- customThe mixture obtained
- concentrationConcentration
- customThe solution obtained
- filtrationAfter filtration and concentration
- customthe residue is chromatographed over silica (eluant CH2Cl2/EtOH: 95/5)
出典と根拠
- ORDレコード
- ord-97fa9183a2d24730a294523322198ffc
- 出典データセット
- uspto-grants-2005_06
- 特許番号
- US06908922B2
関連ノート
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