反应详情

温度

60 °C

To one-half mole of sodium benzenesulfinate in water in a 2 liter beaker is introduced 49 g (0.5 mole) of concentrated sulfuric acid. To the resulting suspension of benzenesulfinic acid is then added 101 g (0.5 mole) of diisopropyl azodicarboxylate. The mixture is stirred and heated to 60° C. (30 minutes). The yellow color of the azo ester gradually disappears. The oily product is extracted with benzene and separated from the lower aqueous layer. Removal of the benzene by evaporation leaves a clear oil which crystallizes when introduced into an 80/20 hexane/benzene mixture. The filtered crystals are dried at 60° C.

1. extractionThe oily product is extracted with benzene
2. customseparated from the lower aqueous layer
3. customRemoval of the benzene
4. customby evaporation
5. customleaves a clear oil which
6. customcrystallizes when
7. additionintroduced into an 80/20 hexane/benzene mixture
8. customThe filtered crystals are dried at 60° C.