反应详情

A mixture of 433E (180 mg, 0.323 mmol) and 1N NaOH (0.68 ml, 0.68 mmol) in EtOH (4 ml) was heated to reflux for 2 days, cooled to rt. Removal of the solvent in vacuo gave a gray oil. Treated with H2O (4 ml), the aqueous solution was washed with EtOAc (3×2 ml) and added to a mixture of 6N HCl (1.5 ml) and brine (5 ml). The resulting suspension was cooled to 0° C. and filtered, dried in vacuo to gave 433F (171 mg, 96%) as a dim dark solid. It has a retention time of 5.31 min (standard LC1 method, 8 min run). MS Found: (M+H)+=530.0

1. temperaturewas heated
2. temperatureto reflux for 2 days
3. customRemoval of the solvent in vacuo
4. customgave a gray oil
5. washthe aqueous solution was washed with EtOAc (3×2 ml)
6. additionadded to a mixture of 6N HCl (1.5 ml) and brine (5 ml)
7. temperatureThe resulting suspension was cooled to 0° C.
8. filtrationfiltered
9. customdried in vacuo