反应详情

A scintillation vial was charged with the product from Example 28 (38 mg, 0.1 mmol), sodium hydroxide (40 mg, 0.1 mmol), hydroxylamine hydrochloride (33 mg, 0.1 mmol) and 4 mL of methanol. The reaction vial was placed in a shaker at room temperature overnight. After this time, the mixture was acidified with 10% HCl, concentrated, and purified on a RP-HPLC to provide the title compound. 1H NMR (500 MHz, DMSO-d6) δ ppm 1.10 (m, 2H), 1.48 (m, 2H), 1.67-1.85 (m, 5H), 1.88 (d, J=6.75 Hz, 2H), 2.47 (m, 1H), 7.12 (s, 1H), 7.34 (d, J=8.28 Hz, 2H), 7.72 (d, J=8.24 Hz, 2H), 8.63 (br s, 1H), 10.34 (s, 1H), 13.96 (br s, 1H); MS (ESI) m/z 366.1 [M−H]+.

1. customThe reaction
2. concentrationconcentrated
3. custompurified on a RP-HPLC