HRID1479844

反应详情

EQUATION

反应方程式

HRID 1479844 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

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-iodoethane (1.2 mol eq, 0.45 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 combined organic phases were dried over Na2SO4 and evaporated under reduced pressure to afford 14A as a pale yellow oil (1.1 g, 98% yield). 1HNMR (DMSO, 200 MHz) δ 1.095 (t, 3H, J=8), 4.43 (bs, 4H), 2.88 (s, 3H), 3.32 (m, 2H), 7.42 (t, 2H, J=8.2), 7.87 (m, 2H).

WORKUP

后处理

  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 combined organic phases were dried over Na2SO4
  5. customevaporated under reduced pressure