反应详情

The mixture from 31.8 g (0.1 mol) of 2-tosyloxymethyl-chroman, 7.1 g (0.07 mol) of anhydrous sodium carbonate and 23.1 g (0.1 mol) of 1-phenyl-1,3,8-triazaspiro[4.5]-decan-4-one in 240 mol of anhydrous dimethylformamide (DMF) is stirred at 110° C. for 6 h and then poured onto ice (500 g). After extracting with ethyl acetate (5×100 ml), washing the organic extracts with water, drying over anhydrous sodium sulphate and evaporating the organic phase in a water jet vacuum, 65.7 g of solvent-containing crystalline crude product are obtained which, recrystallised twice from ethyl acetate, yields 20.6 g of the title compound of m.p. 192-193.5° C.

1. additionpoured onto ice (500 g)
2. extractionAfter extracting with ethyl acetate (5×100 ml)
3. washwashing the organic extracts with water
4. dry with materialdrying over anhydrous sodium sulphate
5. customevaporating the organic phase in a water jet vacuum, 65.7 g of solvent-containing crystalline crude product
6. customare obtained which
7. customrecrystallised twice from ethyl acetate