HRID1986545

反应详情

EQUATION

反应方程式

HRID 1986545 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

81 mg of sodium hydride as a 60% suspension in oil (2.03 μmol) are introduced at room temperature into a 25 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 449 mg (2.03 mmol) of 2-(bromomethyl)naphthalene are then added. The medium is stirred for 16 hours, 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 with 10 ml of water. The organic phase is dried, filtered and then evaporated to dryness to give 1.5 g of crude product, which product is chromatographed on a silica cartridge (25 g) with a 90/10 heptane/EtOAc mixture. 510 mg of product 42 are recovered (yield=65%).

WORKUP

后处理

  1. stirringThe medium is stirred for 1 hour
  2. stirringThe medium is stirred for 16 hours
  3. customafter separation of the phases
  4. washthe organic phase is washed with 10 ml of water
  5. customThe organic phase is dried
  6. filtrationfiltered
  7. customevaporated to dryness