反应详情

温度

60 °C

A solution of 3E (1.4 g, 4.87 mmol) in dioxane (30 mL) was added with 20% NaOH aq. solution (30 mL) and the mixture was heated at 60° C. overnight. The organic solvent was removed under reduced pressure and the aqueous phase was acidified with 10% HCl and extracted with CH2Cl2 (3×50 mL). The combined organic phases were dried over Na2SO4 and evaporated under reduced pressure to afford 4E as a pale yellow solid (0.8 g, 65% yield). 1HNMR (DMSO, 200 MHz) δ 2.81 (s, 3H), 2.88 (s, 3H), 5.46 (s, 1H), 6.02 (s, 2H), 7.41 (d, 2H, J=7.8), 7.66 (d, 2H, H=8), 13.01 (bs, 1H).

1. customThe organic solvent was removed under reduced pressure
2. extractionextracted with CH2Cl2 (3×50 mL)
3. dry with materialThe combined organic phases were dried over Na2SO4
4. customevaporated under reduced pressure