HRID1479864

反应详情

EQUATION

反应方程式

HRID 1479864 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A solution of 3F (3.0 g, 9.8 mmol) in dioxane (30 mL) was added with 20% NaOH aq. solution (20 mL) and the mixture heated at 80° C. for 5 h. The organic solvent was removed under reduced pressure and the aqueous phase acidified with 10% HCl. The solid formed was filtered under vacuum, washed with cold water (1×50 mL) and dried to afford 4F as white solid (650 mg, 25% yield). 1HNMR (DMSO, 200 MHz) δ 1.11 (t, 3H, J=7.7), 3.43 (q, 2H), 5.78 (s, 1H), 6.36 (s, 1H), 7.69 (m, 2H), 7.84 (m, 2H), 12.98 (bs, 1H).

WORKUP

后处理

  1. customThe organic solvent was removed under reduced pressure
  2. customThe solid formed
  3. filtrationwas filtered under vacuum
  4. washwashed with cold water (1×50 mL)
  5. customdried