反应详情

2.0 g of (+/-)-cis-8,9-dimethoxy-6-(4-p-toluenesulfonamidophenyl)-1,2,3,4,4a,10b-hexahydrophenanthridine in 5 ml of dimethylformamide and then 1.0 g of p-toluenesulfonyl chloride in 5 ml of dimethylformamide are added dropwise to a suspension of 200 mg of 80% strength sodium hydride in 20 ml of dimethylformamide. After stirring at RT for 2 h, the mixture is added to ice-water and extracted with ethyl acetate/diethyl ether in the ratio 1:1. After drying and concentration of the organic phase, the residue is chromatographed on silica gel using a mixture of ethyl acetate/petroleum ether in the ratio 4:1. After concentration of the corresponding eluate fractions, the title compound of m.p. 120-130° C. is obtained.

1. extractionextracted with ethyl acetate/diethyl ether in the ratio 1:1
2. customAfter drying
3. customconcentration of the organic phase, the residue is chromatographed on silica gel using
4. additiona mixture of ethyl acetate/petroleum ether in the ratio 4:1