反应详情

温度

120 °C

To a solution of (R)-lysine HCl salt (100 g, 0.68 mol) in xylene (1 L) was added hexamethyldisilazane (1000 mL, 4.76 mol) and chlorotrimethylsilane (10 mL, 78.8 mmol). The mixture was heated to 120° C. for 24 h, then to 180° C. for 48 h. The solvent was then removed under reduced pressure and the crude material was purified by column chromatography (20:1 to 10:1 CH2Cl2/MeOH) to afford (R)-3-aminoazepan-2-one (I-1a).

1. customThe solvent was then removed under reduced pressure
2. customthe crude material was purified by column chromatography (20:1 to 10:1 CH2Cl2/MeOH)