反应详情

温度

90 °C

A mixture of 57 (0.031 g, 0.076 mmol) and 10% aqueous NaOH solution (1 mL) in EtOH (2 mL) was stirred at 90° C. for 1 hour. The mixture was cooled and evaporated to afford a tan syrup. The syrup was dissolved with CH2Cl2 and the solution was washed with brine. The aqueous layer was extracted twice with CH2Cl2. The combined extracts were dried (MgSO4) and concentrated to afford a syrup, which was purified by means of preparative TLC with CH2Cl2:MeOH as eluent to afford 58 (0.016 g, 78%) as a pale brown solid. 1H NMR (400 MHz, CD3OD) δ 3.13-3.17 (m, 4H), 3.85-3.89 (m, 4H), 7.51 (s, 1H), 7.74 (d, J=0.26 Hz, 1H), 7.93 (bs, 2H), 8.06 (d, J=0.26 Hz, 1H).

1. temperatureThe mixture was cooled
2. customevaporated
3. customto afford a tan syrup
4. washthe solution was washed with brine
5. extractionThe aqueous layer was extracted twice with CH2Cl2
6. dry with materialThe combined extracts were dried (MgSO4)
7. concentrationconcentrated
8. customto afford a syrup, which
9. customwas purified by means of preparative TLC with CH2Cl2