反应详情

温度

50 °C

A solution of 13A (1 g, 3.67 mmol) in DMF (15 mL) was added with an. K2CO3 (1.5 mol eq, 0.76 g) and, after few minutes, 2-iodomethane (1.2 mol eq, 0.81 ml) was added and the mixture was heated at 50° C. for 12 h. The solvent was removed under reduced pressure, water was added to the residue (60 mL) and the aqueous phase was extracted with EtOAc (3×30 mL). The recombined organic phases were dried over Na2SO4 and evaporated under reduced pressure to afford 14A as a pale yellow oil (950 mg, 90% yield). 1HNMR (DMSO, 200 MHz) δ 2.43 (bs, 4H), 2.88 (s, 3H), 2.90 (s, 3H), 7.42 (t, 2H, J=8.2), 7.87 (m, 2H).

1. customThe solvent was removed under reduced pressure, water
2. additionwas added to the residue (60 mL)
3. extractionthe aqueous phase was extracted with EtOAc (3×30 mL)
4. dry with materialThe recombined organic phases were dried over Na2SO4
5. customevaporated under reduced pressure