|
|
¡ï koria0727(½ð±Ò+1):¶àл²ÎÓë¡£ 2010-12-04 09:41:49
Intermediate 75. 3-Oxo-3-phenylpropyl acetate; To a solution of 3-chloro-1-phenylpropan-1-one (1.0 g, 5.93 mmol) in acetic acid (8 mL) was added sodium acetate (2.43 g, 29.7 mmol) and potassium iodide (100 mg). The mixture was heated in a sealed tube at 13O0C overnight. After cooling, the reaction was diluted with water (20 mL) and extracted with methylene chloride (3 x 20 mL). The combined organic extracts were washed with water (2 x 50 mL), saturated solution of sodium bicarbonate (2 x 50 mL) and brine (20 mL), dried (Na2SO4), and the solvent removed under reduced pressure. The title compound was obtained (1.0 g, 88percent) as an orange solid. 1H-NMR (300 MHz, CI3CD): 2.03 (s, 3H); 3.32 (t, J=6.0 Hz, 2H); 4.52 (t, J=6.0 Hz, 2H);7.40-7.63 (m, 3H); 7.89-8.02 (m, 2H). MS (M+): 192.
ÏÈÉú³É¡¡ÒÒËáõ¥ÔÙÕÒ·½·¨Ë®½â£¬ÎÒÏëÓ¦¸Ã¿ÉÒÔ°É |
|