HRID1479864
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe organic solvent was removed under reduced pressure
- customThe solid formed
- filtrationwas filtered under vacuum
- washwashed with cold water (1×50 mL)
- customdried