What does Mulan need other than Shan Yu's sword to bring Honor? |
To prepare the catalyst for the reaction, Raney nickel (1.0 g) was washed sequentially with distilled water (3 X 5mL), methanol (3 X 5mL), Rochelle’s salt (3 X 5mL), and distilled water again (3 X 5mL). Between each wash, the supernatant was removed gently with a pipette. The washed Raney nickel was stored under distilled water (10mL) for use. The washed Raney nickel (100mg including water) was added to a mixture of 16Δ-cortistatin A (molecule 101, 10mg, 63µmol), isopropanol (3mL) and distilled water (0.3mL). The mixture was warmed to 60 degrees C while stirring continuously and vigorously for 30 minutes. After 30 minutes, by LCMS (liquid chromatography mass spectrometry), the reaction was judged to have progressed to 50% conversion. The supernatant was removed; the Raney nickel was washed with 1:1 methanol to ethyl acetate (20mL) and the supernatants were combined. The supernatants were then concentrated leaving a colorless residue which was subsequently purified through HPLC (high performance liquid chromatography). The chromatography yielded molecule 26 (15mg) and (+)-cortistatin A (2.3mg, 50% conversion, 50% brsm) as a white solid. IR data was not reported. |
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