反应详情

A mixture of Example 1B (0.175 g, 0.516 mmol) and sodium azide (0.037 g, 0.568 mmol) in N,N-dimethylformamide (5 mL) was heated at 70° C. for 1 hour. The reaction mixture was diluted with water and brine and extracted with ethyl acetate (2×). The combined organic layers were washed with brine (2×), dried over MgSO4, filtered, concentrated, and purified on a 12 g column using the ISCO Companion flash system eluting with CH2Cl2/ethyl acetate (95:5 to 90:10) to provide the title compound.

1. extractionextracted with ethyl acetate (2×)
2. washThe combined organic layers were washed with brine (2×)
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. custompurified on a 12 g column
7. washeluting with CH2Cl2/ethyl acetate (95:5 to 90:10)