反应详情

温度

60 °C

Metachloroperbenzoic acid (0.0501 mol) was dissolved in CHCl3 (40 ml). The organic solution was dried, filtered and the filtrate was added dropwise to a solution of intermediate 1 (0.0417 mol) and 1,4-benzenediol (0.26 g) in CHCl3 (70 ml), stirred at 60° C. The reaction mixture was stirred for 2.5 hours at 60° C., then cooled on an ice-bath, washed with a 10% aqueous Na2CO3 solution and brine, dried, filtered and the filtrate was evaporated, yielding 10.42 g of 3-fluoro-6,10b-dihydro-1aH-dibenzo-[3,4:6,7]cyclohept[1,2-b]oxirene (intermediate 2)

1. customThe organic solution was dried
2. filtrationfiltered
3. stirringThe reaction mixture was stirred for 2.5 hours at 60° C.
4. temperaturecooled on an ice-bath
5. washwashed with a 10% aqueous Na2CO3 solution and brine
6. customdried
7. filtrationfiltered
8. customthe filtrate was evaporated