反应详情

81 mg of sodium hydride as a 60% suspension in oil (2.03 mmol) are introduced at room temperature into a 50 ml round-bottomed flask, with stirring and under an argon atmosphere, containing 20 ml of THF and 500 mg of 26 (2.03 mmol). The medium is stirred for 1 hour and 420 mg (2.03 mmol) of 3,4-difluorobenzyl bromide are then added. The medium is stirred overnight, 20 ml of EtOAc and 20 ml of water are added to the reaction medium and, after separation of the phases by settling, the organic phase is washed once with 20 ml of water. The organic phase is dried, filtered and then evaporated to dryness. 1.5 g of crude product are recovered, which product is chromatographed on silica (eluent: 80/20 heptane/EtOAc). 460 mg of product 30 are recovered (yield=61%).

1. stirringThe medium is stirred for 1 hour
2. stirringThe medium is stirred overnight
3. customafter separation of the phases
4. washthe organic phase is washed once with 20 ml of water
5. customThe organic phase is dried
6. filtrationfiltered
7. customevaporated to dryness
8. custom1.5 g of crude product are recovered
9. customwhich product is chromatographed on silica (eluent: 80/20 heptane/EtOAc)
10. custom460 mg of product 30 are recovered (yield=61%)