反应详情

温度

50 °C

A solution of 2G (2.85 g, 8.8 mmol) in DMF (20 mL) was added with an. K2CO3 (1.5 mol eq, 1.83 g) and, after few minutes, 2-iodoethane (1.2 mol eq, 1.09 mL) was added and the mixture heated at 50° C. for 12 h. The solvent was removed under reduced pressure, water was added to the residue (150 mL) and the aqueous phase extracted with EtOAc (3×60 mL). The recombined organic phases were dried over Na2SO4 and evaporated under reduced pressure to afford 3G as a pale yellow oil (2.8 g, 90% yield). 1HNMR (DMSO, 200 MHz) δ 1.15 (m, 3H), 1.98 (s, 3H), 3.08 (m, 2H), 4.04 (q, 2H, J=8), 4.58 (t, 1H), 5.15 (bm, 1H), 7.71 (m, 2H), 7.94 (m, 1H).

1. customThe solvent was removed under reduced pressure, water
2. additionwas added to the residue (150 mL)
3. extractionthe aqueous phase extracted with EtOAc (3×60 mL)
4. dry with materialThe recombined organic phases were dried over Na2SO4
5. customevaporated under reduced pressure