反应详情

温度

80 °C

A solution of 3C (8.5 g, 27.6 mmol) in dioxane (20 mL) was added with 20% NaOH aq. solution (30 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 and extracted with CH2Cl2 (3×50 mL). The combined organic phases were dried over Na2SO4 and evaporated under reduced pressure to afford 4C as a pale yellow deliquescent solid (4.3 g, 62% yield). 1HNMR (DMSO, 200 MHz) δ 2.91 (s, 3H), 5.58 (s, 1H), 6.09 (s, 1H), 7.72-7.60 (m, 4H), 13.05 (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