反应详情

温度

115 °C

To a solution of (3aR,7S,7aS)-7-(4-amino-3-fluoro-5-iodo-benzyl)-3-(3-tert-butyl-benzyl)-5,5-dioxo-hexahydro-1-oxa-5lambda*6*-thia-3-aza-inden-2-one (0.10 g, 0.17 mmol), 2-pyrrolidin-one (0.02 mL, 0.26 mmol) and N,N′-dimethylethylenediamine (0.002 mg, 0.017 mmol) in dioxane (10 mL) was added CuI (0.002 g, 0.009 mmol) and K3PO4 (0.077 g, 0.36 mmol) and the reaction mixture was heated at 115° C. for 4 h. The reaction mixture was filtered over Celite and concentrated. The crude product was purified on the flashmaster (10 g silicagel, cyclohexane-EtOAc 100:0 to 0:100) to yield the title compound as a yellow solid, which was directly used as such in the next step: HPLC RtC=4.728 min; ESIMS [M+H]+=544.

1. filtrationThe reaction mixture was filtered over Celite
2. concentrationconcentrated
3. customThe crude product was purified on the flashmaster (10 g silicagel, cyclohexane-EtOAc 100:0 to 0:100)