反应详情

The product of Example 48 (300 mg, 0.67 mmol) and trifluoroethylamine (300 mg, 3 mmol) were dissolved in THF (10 ml) and sealed in a vial under Ar. The mixture was heated in an oil bath to 60° for 4 days. The solvents were removed in vacuo, and the residue was flash chromatographed with 60-90% CH2Cl2/hexane. Recrystallization from CH2Cl2/hexane gave the title compound as a white crystalline solid. mp 195-196°, LC MS m/z=465(MH+) Retention time=2.38 min.

1. customsealed in a vial under Ar
2. temperatureThe mixture was heated in an oil bath to 60° for 4 days
3. customThe solvents were removed in vacuo
4. customchromatographed with 60-90% CH2Cl2/hexane
5. customRecrystallization from CH2Cl2/hexane