反应详情

0.09 cm3 of triethylamine is added to a suspension of 0.25 g of 6,6-diphenyl-1-(4-toluenesulphonyl)-6,7-dihydro-1H-indazol-3-carboxylic acid in 1.5 cm3 of toluene and 1.5 cm3 of tert-butanol. The solution obtained is heated to the reflux temperature and 0.12 cm3 of diphenylphosphonyl azide is added dropwise. Refluxing of the reaction mixture is continued for eight hours. After forty-eight hours at a temperature in the region of 20° C., the reaction mixture is concentrated to dryness under reduced pressure (13 kPa) and the residue is purified by flash chromatography on a column of silica [eluent: dichloromethane]. 0.06 g of tert-butyl [6,6-diphenyl-1-(4-toluenesulphonyl)-6,7-dihydro-1H-indazol-3-yl]carbamate is thus obtained in the form of a white foam, which is used directly, the characteristics of which are as follows:

1. customThe solution obtained
2. additionis added dropwise
3. temperatureRefluxing of the reaction mixture
4. waitAfter forty-eight hours at a temperature in the region of 20° C.
5. concentrationthe reaction mixture is concentrated to dryness under reduced pressure (13 kPa)
6. customthe residue is purified by flash chromatography on a column of silica [eluent: dichloromethane]