3-Chloropropiophenone synthesis
- Product Name:3-Chloropropiophenone
- CAS Number:936-59-4
- Molecular formula:C9H9ClO
- Molecular Weight:168.62
Yield:936-59-4 100%
Reaction Conditions:
with aluminum (III) chloride in dichloromethane at 0 - 20;Inert atmosphere;
Steps:
31 Example 31 :3-Chloro-1 -phenylpropane-1 -one (50).
3-Chloropropionyl chloride (0.151 g; 1.19 mmol) followed by anhydrous benzene (0.084 g; 1.08 mmol) were added in a dropwise fashion to a solution of aluminum trichloride(0.173 g; 1.30 mmol) dissolved in anhydrous CH2CI2 (1 ml_), under N2 atmosphere at 0°C. The reaction mixture was allowed to warm to room temperature and left overnight.The reaction mixture was then cooled to 0°C and quenched by lumps of ice. The aqueous phase was extracted with CH2CI2 and the combined organic phases were dried over MgS04, filtered and concentrated. The product was purified by column chromatography (pentane) and isolated as yellow crystals in quantitative yield (0.200 g;1.19 mmol).Rf (pentane) 0.31. Mp (uncorr.): 45.9-48.7°C. 1H-NMR (400 MHz, CDCI3) δΗ 8.00-7.93 (m, 2H), 7.64-7.55 (m, 1 H), 7.53-7.44 (m, 2H), 3.93 (t, 2H, J 6.8 Hz), 3.46 (t, 2H, J 6.8 Hz). 13C-NMR (100 MHz, CDCI3) 5C 196.8, 136.5, 133.7, 128.9, 128.2, 41.4, 38.8. The NMR data are in accordance with those previously reported (Moriyama, K.;Takemura, M.; Togo, H. Org. Lett. 2012, 14, 2414-2417).
References:
WO2013/26455,2013,A1 Location in patent:Page/Page column 74
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