反应详情

温度

90 °C

A mixture of sodium ethanethiolate (151 mg, 1.79 mmol) and 24 (150 mg, 0.179 mmol) in DMF (3 mL) was flushed with argon and heated at 90° C. for 3 h. The reaction mixture was cooled to 0° C. A mixture of acetic acid and water (1:1, 2 mL) was added. The resulting mixture was stirred for 10 min and then concentrated to dryness. The residue was partitioned between water and dichloromethane. The organic layer was separated, dried (Na2SO4), and evaporated. The residue was purified by preparatory TLC eluting with 10% EtOAc in petroleum ether to give 25 (135 mg, 92%). LC/MS m/z 846 (M+Na).

1. customwas flushed with argon
2. temperatureThe reaction mixture was cooled to 0° C
3. additionA mixture of acetic acid and water (1:1, 2 mL)
4. additionwas added
5. concentrationconcentrated to dryness
6. customThe residue was partitioned between water and dichloromethane
7. customThe organic layer was separated
8. dry with materialdried (Na2SO4)
9. customevaporated
10. customThe residue was purified by preparatory TLC
11. washeluting with 10% EtOAc in petroleum ether