反应详情

In 22.4 g of dimethylformamide were dissolved 22.5 g (0.050 mol) of the bis(4-n-pentylcyclohexylsulfonyl)methane prepared above and 14.8 g (0.075 mol) of p-toluenesulfonylazide. To this solution were added 90.1 g of ethanol and 22.2 g of water. The solution was cooled on an ice bath, to which 2.0 g (0.050 mol) of sodium hydroxide in 23 g of water was added dropwise at a temperature below 5° C. The solution was ripened at the temperature for 6.5 hours. Filtration of the crystals gave 2.6 g of the desired bis(4-n-pentylcyclohexylsulfonyl)diazomethane. The yield was 46%.

1. additionwas added dropwise at a temperature below 5° C
2. filtrationFiltration of the crystals