反应详情

温度

70 °C

A mixture of [(4-nitro-phenyl)-ethoxy-phosphinoylmethyl]-phosphonic acid diethyl ester (940 mg, 2.57 mmol) and SnCl2.2H2O (2.9 g, 12.9 mmol) in EtOH (˜10 mL) was stirred at 70° C. for 44 min and then concentrated at ambient temperature. The residue was taken up in CH2Cl2 and washed with half saturated aq NaHCO3 (40 mL), H2O (40 mL) and brine (40 mL). The aqueous washes were reextracted once with CH2Cl2, and the combined extracts were dried over K2CO3 and concentrated. The crude material was purified by flash chromatography on silica gel. Elution with 20:1 CHCl3-MeOH followed by 15:1 CHCl3-MeOH afforded 657 mg of product.

1. concentrationconcentrated at ambient temperature
2. washwashed with half saturated aq NaHCO3 (40 mL), H2O (40 mL) and brine (40 mL)
3. dry with materialthe combined extracts were dried over K2CO3
4. concentrationconcentrated
5. customThe crude material was purified by flash chromatography on silica gel
6. washElution with 20:1 CHCl3-MeOH