反应详情

A mixture of the Compound of Example 3 (500 mg, 2.36 mmol), 3-methyl-1,2-cyclopentanedione (350 mg, 3.11 mmol), acetic acid (0.18 mL, 3.11 mmol) in ethanol (10 mL) was refluxed for 8 h. The reaction mixture was evaporated, poured into water and extracted with EtOAc. The combined organic layers were washed with brine, dried on Na2SO4 and evaporated to dryness in vacuo to afford a residue, which was purified by automated flash liquid chromatography (Horizon™-Biotage) eluting with Petroleum Ether-EtOAc 85:15, affording the title product as a brown solid.

1. temperaturewas refluxed for 8 h
2. customThe reaction mixture was evaporated
3. additionpoured into water
4. extractionextracted with EtOAc
5. washThe combined organic layers were washed with brine
6. customdried on Na2SO4
7. customevaporated to dryness in vacuo
8. customto afford a residue, which
9. customwas purified by automated flash liquid chromatography (Horizon™-Biotage)
10. washeluting with Petroleum Ether-EtOAc 85:15