反应详情

To a solution of the product of Step 2 (8.01 g, ca. 30 mmol) in dichloromethane (100 ml) at 0° C. was added cyclopropylamine (4.16 ml, 60 mmol) drop-wise. The resulting mixture was stirred overnight at room temperature, then concentrated under vacuum to a residue and re-dissolved in ethyl acetate, basifying with sodium bicarbonate. The organic phase was washed with water three times, followed by twice with brine before concentrating under vacuum to a crude solid. This oil was purified by column chromatography eluting with a gradient of 50% DCM/hexane to DCM affording product as a yellow solid, 6.22 g (80%); MS (ES+) m/e 258/260 [M+H]+.

1. concentrationconcentrated under vacuum to a residue
2. dissolutionre-dissolved in ethyl acetate
3. washThe organic phase was washed with water three times
4. concentrationbefore concentrating under vacuum to a crude solid
5. customThis oil was purified by column chromatography
6. washeluting with a gradient of 50% DCM/hexane to DCM affording product as a yellow solid, 6.22 g (80%)