反应详情

温度

80 °C

A solution of 3B (1.1 g, 3.6 mmol) in dioxane (25 mL) was added with 20% NaOH aq. solution (20 mL) and the mixture heated at 80° C. for 4 h. The organic solvent was removed under reduced pressure and the aqueous phase acidified with 10% HCl and extracted with CH2Cl2 (3×30 mL). The combined organic phases were dried using Na2SO4, evaporated under reduced pressure and then the resulting residue purified by flash chromatography (100% EtOAc) to obtain 4B as white solid (0.7 g, 66% yield). 1HNMR (DMSO, 200 MHz) δ 1.12 (t, 3H), 3.29 (q, 2H), 5.69 (s, 1H), 6.32 (s, 1H), 7.39 (m, 2H), 7.89 (m, 2H), 12.9 (bs, 1H).

1. customThe organic solvent was removed under reduced pressure
2. extractionextracted with CH2Cl2 (3×30 mL)
3. customThe combined organic phases were dried
4. customevaporated under reduced pressure
5. customthe resulting residue purified by flash chromatography (100% EtOAc)