反应详情

The product of step 3 of Example 4 (10 mg, 0.025 mmol) is stirred with concentrated sulfuric acid (0.5 mL) at room temperature for 30 minutes. The solution is basified with saturated aqueous sodium bicarbonate (5 mL) and extracted with 10% methanol in CH2Cl2 (10 mL). The organics are concentrated and the residue purified by chromatography on a reverse phase C-18 column eluting with a gradient of neat water with 0.1% trifluoroacetic acid to neat acetonitrile with 0.1% trifluoroacetic acid to give the title compound (2 mg): m/z (Cl) 415 [M+H].

1. extractionextracted with 10% methanol in CH2Cl2 (10 mL)
2. concentrationThe organics are concentrated
3. customthe residue purified by chromatography on a reverse phase C-18 column
4. washeluting with a gradient of neat water with 0.1% trifluoroacetic acid to neat acetonitrile with 0.1% trifluoroacetic acid