反应详情

温度

40 °C

Compound 78 (0.100 g, 0.189 mmol) was dissolved in DCM (3 mL) followed by TFA (1 mL) and stirred at 40° C. in a water bath for 30 min. Concentration under vacuum provided a yellowish oil which was partially dissolved in water and then filtered. The filtrate was purified by preparative RP-HPLC eluting with a gradient of 5% MeCN/water/0.1% TFA-30% MeCN/water/0.1% TFA to yield compound 76 as a yellow solid (33 mg). 1H NMR (500 MHz, DMSO-d6) δ 10.18 (1H, s), 9.51 (1H, s), 9.31 (1H, s), 8.95 (2H, br s), 8.65 (1H, d, J=6.2 Hz), 8.55 (1H, d, J=6.1 Hz), 8.12 (1H, d, J=3.0), 7.58 (1H, d, J=2.4 Hz), 5.25 (1H, p, J=8.3 Hz), 3.46 (4H, t, J=5.4 Hz), 3.30 (4H, m), 2.24 (3H, s), 2.18 (2H, m), 2.01 (2H, m), 1.70 (2H, m), 1.55 (2H, m) ppm; LCMS-ESI (POS), M/Z, M+1: Found 429.2.

1. concentrationConcentration under vacuum
2. customprovided a yellowish oil which
3. filtrationfiltered
4. customThe filtrate was purified by preparative RP-HPLC
5. washeluting with a gradient of 5% MeCN/water/0.1% TFA-30% MeCN/water/0.1% TFA