反应详情

Intermediate 11 (12.46 g; 47.13 mmol) was dissolved in DCM (200 mL) and n,n′-dicyclohexylcarbodiimide (11.67 g; 56.56 mmol) was added. Then Intermediate 1 was added (10 g; 47.13 mmol) and the suspension was stirred at RT for 12 hours. The precipitate was filtered off and the solvent evaporated to give a yellow solid. The residue was dissolved in Toluene (300 mL) and Py (150 mL) and the solution was heated to 130° C. for 12 hours. The reaction mixture was concentrated to afford a yellow sticky oil which was precipitated from ACN affording the title compound as a yellow solid. LC/MS (Method B): 441.3 (M+H)+ HPLC: Rt 5.86 min (Purity: 95.1%).

1. filtrationThe precipitate was filtered off
2. customthe solvent evaporated
3. customto give a yellow solid
4. temperaturePy (150 mL) and the solution was heated to 130° C. for 12 hours
5. concentrationThe reaction mixture was concentrated
6. customto afford a yellow sticky oil which
7. customwas precipitated from ACN affording the title compound as a yellow solid