反应详情

A mixture of Example 1B (0.150 g, 0.442 mmol) and acetohydrazide (0.072 g, 0.973 mmol) in acetonitrile (5 mL) was heated at 150° C. for 15 minutes in a Biotage microwave reactor. The solid was filtered. The filtrate was concentrated, treated with saturated aqueous NaHCO3 and extracted with ethyl acetate (2×). The combined organic layers were dried over MgSO4, filtered, concentrated, and purified on a 12 g column using the ISCO Companion flash system eluting with CH2Cl2/ethyl acetate (3:7 to 2:8) to provide the title compound.

1. filtrationThe solid was filtered
2. concentrationThe filtrate was concentrated
3. additiontreated with saturated aqueous NaHCO3
4. extractionextracted with ethyl acetate (2×)
5. dry with materialThe combined organic layers were dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. custompurified on a 12 g column
9. washeluting with CH2Cl2/ethyl acetate (3:7 to 2:8)