反应详情

温度

80 °C

The crude diketone (1.17 g) from step 3 was dissolved in acetic acid (14 mL) and the solution was diluted with aqueous 6N HCl (14 mL). The resulting mixture was stirred and heated in an oil bath at 80° C. for 5 hours and then kept at room temperature for 3 days. The mixture was diluted with EtOAc (100 mL) and carefully basified with aqueous K2CO3 (200 mL). The organic portion was washed with brine, dried over MgSO4 filtered, and evaporated under vacuum. The residue was lyophilized from benzene to afford crude 7-amino-8-bromo-9a-ethyl-4-methyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one (1.0 g) as an amorphous solid.

1. washThe organic portion was washed with brine
2. dry with materialdried over MgSO4
3. filtrationfiltered
4. customevaporated under vacuum