反应详情

温度

107 °C

A solution of amino(chloro)methylaluminum (0.5 M in toluene, 18.13 mL, 9.06 mmol) was added quickly to a stirred solution of the intermediate from Step F (0.3006 g, 1.036 mmol) in toluene (12.63 mL) and the mixture was heated at 107° C. overnight. The reaction mixture was cooled to room temperature, MeOH was added and the mixture was stirred for 30 min. The reaction mixture was filtered through a plug of Celite™ (diatomaceous earth), washed through with 2M NH3 in MeOH and the filtrate was concentrated in vacuo to give the crude product. This was purified by flash chromatography using a DCM/MeOH (2 N NH3 in MeOH) gradient to afford the desired product, as a yellow solid. m/z=308.0 (M+H).

1. temperatureThe reaction mixture was cooled to room temperature
2. filtrationThe reaction mixture was filtered through a plug of Celite™ (diatomaceous earth)
3. washwashed through with 2M NH3 in MeOH
4. concentrationthe filtrate was concentrated in vacuo
5. customto give the crude product
6. customThis was purified by flash chromatography