反应详情

温度

60 °C

A solution of Intermediate 153i (131 mg, 0.13 mmol) in THF (0.8 mL) was treated with a 2M solution of dimethylamine in THF (1.3 mL, 2.6 mmol) and the mixture was stirred at 60° C. for 18 h. The cooled solution was concentrated in vacuo, and the residue was partitioned between DCM and water. The phases were separated and the aqueous layer was extracted with DCM (×2). The combined organic phase was washed with brine, dried (Na2SO4) and concentrated in vacuo to a brown gum. The gum was purified by FCC, using 0-8% (2N NH3MeOH) in DCM, to give the title compound as a white foam (93 mg, 75%). LCMS (Method 3): Rt 3.91 min, m/z 960.6 [MH+].

1. concentrationThe cooled solution was concentrated in vacuo
2. customthe residue was partitioned between DCM and water
3. customThe phases were separated
4. extractionthe aqueous layer was extracted with DCM (×2)
5. washThe combined organic phase was washed with brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated in vacuo to a brown gum
8. customThe gum was purified by FCC