反应详情

A mixture of Example 9E (8.7 g, 28.8 mmol) and 6 N NaOH aqueous (20 mL) in MeOH (100 mL) was stirred at 50° C. overnight, cooled to room temperature, and concentrated under reduced pressure. The residue was diluted with water and extracted with CH2Cl2 (3×100 mL). The combined organic extracts were washed with brine and concentrated to provide 5.3 g (89%) of the title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm 0.37-0.44 (m, 2H), 0.47-0.54 (m, 2H), 1.07-1.20 (m, 1H), 1.29-1.36 (m, 9H), 3.78 (s, 3H), 4.10 (d, J=6.74 Hz, 2H), 5.60 (s, 1H), 7.19 (s, 1H); MS (+DCI) m/z 208 [M+H]+.

1. concentrationconcentrated under reduced pressure
2. additionThe residue was diluted with water
3. extractionextracted with CH2Cl2 (3×100 mL)
4. washThe combined organic extracts were washed with brine
5. concentrationconcentrated