반응 #73464

반응 방정식

1-(4-Fluoro-phenyl)-4-oxo-cyclohexanecarbonitrile

toluene

p-toluene sulfonic acid

→

desired product

8-(4-Fluoro-phenyl)-1,4-dioxa-spiro[4.5]decane-8-carbonitrile

반응 조건

후처리

1. 1
   온도the reaction mixture was heated in a Dean-Stark apparatus for 6 h
2. 2
   세척washed twice with saturated aqueous sodium bicarbonate solution and brine
3. 3
   건조dried over magnesium sulphate
4. 4
   기타evaporated to dryness

실험 절차

15 g of 1-(4-Fluoro-phenyl)-4-oxo-cyclohexanecarbonitrile (12) were dissolved in 500 mL of toluene, then 900 mg of p-toluene sulfonic acid were added and the reaction mixture was heated in a Dean-Stark apparatus for 6 h. The mixture was allowed to cool to room temperature and washed twice with saturated aqueous sodium bicarbonate solution and brine, dried over magnesium sulphate and evaporated to dryness to yield 17.9 g of the desired product. Rt=1.47 min (Method 5). Detected mass: 262.2 (M+H+).

출처