反应详情

Trichloroethyl chloroformate (0.1 mL, 0.78 mmol) was added to a solution of Intermediate 3b (176 mg, 0.60 mmol) and DIPEA (0.31 mL, 1.81 mmol) in THF (10 mL), and the mixture stirred for 3 h. The mixture was then partitioned between water (15 mL) and EtOAc (3×20 mL), and the combined organic extracts dried (Na2SO4) and concentrated in vacuo. The residue was triturated (cyclohexane) and filtered to give the title compound as a yellow solid (280 mg, 100%). LCMS (Method 1): Rt 3.93 min, m/z 466/468 [MH+]

1. customThe mixture was then partitioned between water (15 mL) and EtOAc (3×20 mL)
2. dry with materialthe combined organic extracts dried (Na2SO4)
3. concentrationconcentrated in vacuo
4. customThe residue was triturated (cyclohexane)
5. filtrationfiltered