反应详情

温度

50 °C

A mixture of 3-bromo-1,1-diethoxy-propan-2-one (21.3 g, 95 mmol) (Step 179.9) and N-tert-butoxycarbonylguanidine (45.3 g, 284 mmol, 3 equiv) (Step 179.10) was stirred at 50° C. for 8 h. The reaction mixture was concentrated, diluted in EtOAc/H2O and extracted with EtOAc. The organic phase was washed with water and brine, dried (Na2SO4) and concentrated. The residue was purified by silica gel column chromatography (DCM/EtOAc, 3:7) followed by trituration in Et2O to afford 11.3 g of the title compound as a white solid: ES-MS: 286 [M+H]+; Rf=0.34 (DCM/EtOAc, 3:7).

1. concentrationThe reaction mixture was concentrated
2. additiondiluted in EtOAc/H2O
3. extractionextracted with EtOAc
4. washThe organic phase was washed with water and brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated
7. customThe residue was purified by silica gel column chromatography (DCM/EtOAc, 3:7)