反应详情

温度

80 °C

The product of Example 1, step (d) (75 mg, 0.33 mmol) was dissolved in 2 mL DCE and treated with phenyl sulfonyl chloride (83 uL, 0.66 mmol) followed by AlCl3 (88 mg, 0.66 mmol). After heating to 80° C. for ½ hour, the reaction was cooled and quenched carefully with 1M NaOH. The product was extracted into DCM (2×). The organic extracts were concentrated and the residue was dissolved in 3 mL each EtOH and 40% aqueous KOH. The reaction was heated to 100° C. for 14 hours, cooled, and diluted with water. The title compound was extracted into DCM (2×5 mL) and purified by preparative HPLC-MS. 1H NMR (CD3OD) δ 7.96 (d, J=8.1 Hz, 2H), 7.67-7.56 (m, 3H), 5.56 (s, 1H), 3.38-3.32 (m, 4H), 3.27-3.23 (m, 2H), 3.09 (t, J=5.4 Hz, 2H); MS: ESI (positive): 294 (M+H).

1. temperaturethe reaction was cooled
2. customquenched carefully with 1M NaOH
3. extractionThe product was extracted into DCM (2×)
4. concentrationThe organic extracts were concentrated
5. dissolutionthe residue was dissolved in 3 mL each EtOH
6. temperatureThe reaction was heated to 100° C. for 14 hours
7. temperaturecooled
8. additiondiluted with water
9. extractionThe title compound was extracted into DCM (2×5 mL)
10. custompurified by preparative HPLC-MS