反应详情

The product from Example 250, Part 4 (174 mg, 0.644 mmol) and cyclopropylamine (35.6 mg, 0.611 mmol) were dissolved in methanol (6.0 mL). That solution was treated with acetic acid (0.209 mL) and sodium cyanoborohydride (38.4 mg, 0.611 mmol). The reaction mixture was stirred at rt overnight. It was concentrated, diluted with ethyl acetate and washed with a saturated NaHCO3 solution. The organic layer was dried over MgSO4, filtered and concentrated. The residue was flash chromatographed (silica, 5% to 6% to 10% MeOH/CH2Cl2) to provide the desired product as a colorless oil (131 mg, 68.8% yield). LCMS: m/z 312.2 (M+H)+.

1. concentrationIt was concentrated
2. additiondiluted with ethyl acetate
3. washwashed with a saturated NaHCO3 solution
4. dry with materialThe organic layer was dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. customchromatographed (silica, 5% to 6% to 10% MeOH/CH2Cl2)