反应详情

30 ml (48 mmol) of 1.6 M BuLi are added dropwise at −78° C. to a solution of 15.8 g (44 mmol) of 7 in 132 ml of dry THF. After 15 minutes, 16 g (57.2 mmol) of 1,2-diiodoethane are added as solid, and the mixture is allowed to warm to room temperature over the course of 1 hour. Water and methyl tert-butyl ether are subsequently added. The organic phase is washed with water, sat. Na2S2O5 and sat. NaCl, dried over MgSO4 and filtered through SiO2. The solvent is removed under reduced pressure, petroleum ether is added to the oily residue, and the product is recrystallised at −25° C. (yield: 84%, m.p. 76.0° C.).

1. washThe organic phase is washed with water, sat. Na2S2O5 and sat. NaCl
2. dry with materialdried over MgSO4
3. filtrationfiltered through SiO2
4. customThe solvent is removed under reduced pressure, petroleum ether
5. additionis added to the oily residue
6. customthe product is recrystallised at −25° C. (yield: 84%, m.p. 76.0° C.)