반응 #2358529

반응 방정식

water

1-Chloroacetone

3-fluoro-5-methylsulfonyl-phenol

potassium carbonate

→

1-(3-fluoro-5-methylsulfonyl-phenoxy)propan-2-one

용매

dimethyl formamide

반응 조건

후처리

1. 1
   온도to cool to ambient temperature
2. 2
   추출The aqueous phase was extracted with ethyl acetate (3×100 ml)
3. 3
   세척the combined organic phase was washed with LiCl (5% aqueous solution, 4×50 ml), brine (50 ml)
4. 4
   건조dried with Na2SO4
5. 5
   기타evaporated
6. 6
   기타Purification on flash chromatography (isooctane:ethyl acetate 1:0 to 3:2)

실험 절차

1-Chloroacetone (95%, 2.66 g, 27.34 mmol) was added to a stirred solution of 3-fluoro-5-methylsulfonyl-phenol (80%, 1.3 g, 5.46 mmol) and potassium carbonate (2.26 g, 16.40 mmol) in dry dimethyl formamide (10 ml), the mixture was heated to 120° C. for 20 minutes, the mixture was allowed to cool to ambient temperature and water (100 ml) was added. The aqueous phase was extracted with ethyl acetate (3×100 ml), the combined organic phase was washed with LiCl (5% aqueous solution, 4×50 ml), brine (50 ml) and dried with Na2SO4 and evaporated. Purification on flash chromatography (isooctane:ethyl acetate 1:0 to 3:2). 0.905 g, 67%. MS m/z (relative intensity, 70 eV) 246 (M+, 79), 204 (55), 203 (bp), 141 (30), 94 (67).

출처