反应详情

A solution of benzoyl chloride (0.73 g, 5.0 mmol) in dichloromethane was added slowly to a solution of tetraethyl 5-aminopentane-1,1-bisphosphonate (1.50 g, 4.5 mmol) from Example 11, part A, and triethylamine (0.76 mL, 5.5 mmol) in dichloromethane at 0° C. After warming to room temperature for 30 minutes, the reaction was quenched by addition of 1N HCl (30 mL). The product was extracted into dichloromethane (2×20 mL) and the combined organic layers were washed with saturated NaHCO3 (2×15 mL), dried (Na2SO4), and concentrated in vacuo. Flash chromatography on silica gel eluting with 15% i-propanol in ethylacetate in EtOAc gave the title compound (0.64 g) as an oil.

1. customthe reaction was quenched by addition of 1N HCl (30 mL)
2. extractionThe product was extracted into dichloromethane (2×20 mL)
3. washthe combined organic layers were washed with saturated NaHCO3 (2×15 mL)
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated in vacuo