反应详情

温度

35 °C

To a solution of Example 150a (0.500 g, 0.990 mmol) in CH2Cl2 (9 mL) was added trifluoroacetic acid (4 mL, 51.9 mmol). The mixture was heated at 35° C. for 6 hours and concentrated. The residue was treated with saturated NaHCO3 and extracted with EtOAc. The organic layer was concentrated. The crude was triturated with EtOAc/diethyl ether to give 222 mg of the title compound. The filtrate was concentrated and purified on a 12 g column using the ISCO Companion flash system eluting with CH2Cl2/EtOAc (95:5 to 90:10) to give more title compound (84 mg).

1. concentrationconcentrated
2. additionThe residue was treated with saturated NaHCO3
3. extractionextracted with EtOAc
4. concentrationThe organic layer was concentrated
5. customThe crude was triturated with EtOAc/diethyl ether