反应详情

温度

0 °C

1.06 g of product obtained in Stage C is dissolved in 28 cm3 of toluene, then the reaction medium is cooled down to 0° C. and 337 μl of diphosgene is added under an inert gas. The temperature is allowed to rise and is maintained at 20° C. for 2 hours. Concentration is carried out under reduced pressure then the residue is chromatographed on silica eluting successively with methylene chloride-acetone 95/5 then 80/20 and finally methylene chloride-methanol, triethylamine 92/8/3 and 362 mg of expected product C13H16N2O (M=216.85 g) is obtained i.e. a yield of 30%.

1. temperatureis maintained at 20° C. for 2 hours
2. concentrationConcentration
3. customthe residue is chromatographed on silica eluting successively with methylene chloride-acetone 95/5