反应详情

2.42 g (0.01 mol) of the 1-(2',2',2'-trichloroethyl)spiro(3.3)heptan-2-one produced according to Example 10 is placed into 30 ml of methylene chloride, and 2 g (0.012 mol) of m-chloroperbenzoic acid is added. The reaction mixture is subsequently stirred for 48 hours at room temperature (21°-26° C.), filtered, and then washed with methylene chloride. The filtrate is washed with cold (0°-5° C.) sodium carbonate solution and cold (0°-5° C.) water, dried over sodium sulphate and concentrated by evaporation. The residue is recrystallised from diethyl ether/n-hexane to yield 5-(2',2',2'-trichloroethyl)-6-oxaspiro(3.4)octan-7-one of the formula ##STR14## as white crystals, m.p. 86.5°-87.5° C.

1. additionis added
2. filtrationfiltered
3. washwashed with methylene chloride
4. washThe filtrate is washed with cold (0°-5° C.) sodium carbonate solution and cold (0°-5° C.) water
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated by evaporation
7. customThe residue is recrystallised from diethyl ether/n-hexane