反应详情

1.352 g of (2,4 dinitro-1-naphthylamino)-methanephosphonic acid diethyl ester is dissolved in 32 ml of ethanol and 23 ml of water, to it is added 4.4 ml of 25% ammonium hydroxide solution, 1.61 g of ammonium chloride and 2.81 g of 35% sodium sulfide and the solution is heated for a few hours to 90° C. The ethanol-water mixture is concentrated by evaporation on a rotary evaporator, taken up in water, extracted with ethyl acetate, washed with brine, dried and spun in. The crude product is chromatographed on silica gel with 2 liters of cyclohexane and ethyl acetate 1:1 and 1 liter of pure ethyl acetate as mobile solvent. 262 mg of product is obtained in several fractions as brown solid.

1. temperaturethe solution is heated for a few hours to 90° C
2. concentrationThe ethanol-water mixture is concentrated by evaporation on a rotary evaporator
3. extractionextracted with ethyl acetate
4. washwashed with brine
5. customdried
6. customThe crude product is chromatographed on silica gel with 2 liters of cyclohexane and ethyl acetate 1:1 and 1 liter of pure ethyl acetate as mobile solvent