HRID1986539

反应详情

EQUATION

反应方程式

HRID 1986539 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

121 mg of sodium hydride as a 60% suspension in oil (3.05 mmol) are introduced at room temperature into a 50 ml round-bottomed flask, with stirring and under an argon atmosphere, containing 20 ml of DMF and 500 mg of 26 (2.03 mmol). The medium is stirred for 1 hour and 454 mg (2.03 mmol) of 3,5-difluorobenzyl bromide are then added. The medium is stirred for 3 hours, 50 ml of EtOAc and 50 ml of water are added to the reaction medium and, after separation of the phases by settling, the organic phase is washed with 50 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 a silica cartridge (20 g, eluent: 80/20 heptane/EtOAc). 600 mg of product 33 are recovered (yield=79%).

WORKUP

后处理

  1. stirringThe medium is stirred for 1 hour
  2. stirringThe medium is stirred for 3 hours
  3. customafter separation of the phases
  4. washthe organic phase is washed with 50 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 a silica cartridge (20 g, eluent: 80/20 heptane/EtOAc)
  10. custom600 mg of product 33 are recovered (yield=79%)