反应详情

Tin(II) chloride dihydrate (400 mg, 1.77 mmol) was added to a solution of 3 (55 mg, 0.0715 mmol) in THF (1 mL) and ethanol (1.5 mL). The reaction mixture was heated at reflux for 3 days, then allowed to cool down to room temperature. Then, volatiles were evaporated under vacuum and the residue was successively partitioned between a diluted solution of NaHCO3 and ethyl acetate, dried (Na2SO4) and evaporated. Purification by column chromatography (CH2Cl2/methanol, 97.5:2.5) afforded the title compound 4 as a yellowish powder: m/z=740 (M+H)+.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 3 days
3. customThen, volatiles were evaporated under vacuum
4. customthe residue was successively partitioned between a diluted solution of NaHCO3 and ethyl acetate
5. dry with materialdried (Na2SO4)
6. customevaporated
7. customPurification by column chromatography (CH2Cl2/methanol, 97.5:2.5)