| 摘要 |
Loxoprofen sodium pharmaceutical intermediates 2-chloro-1-p-tolyl-1-propanone synthesis method comprises the following steps: equipped with a stiffer, a thermometer , a reflux condenser and a dropping funnel, the reaction vessel was added stannous chloride 2.4-2.43mol, 1.2 L toluene solution, the temperature of the solution is reduced to 2- 5 C, added 2.1 mol 2-chloride propionamide solution, dropwise time control for 3-4h, maintaining the stirring speed 180-210rpm, sustained 9-10h, the reaction solution was poured into 2L sodium chloride solution, the solution temperature is reduced to 2--4 C separated the organic layer, the aqueous layer was extracted 3-6 times with toluene solution, and the combined organic layer was successively washed with sodium carbonate solution, saline solution, distilled under reduced pressure to recover the solvent to got oil, the temperature of the solution is reduced to 12 - 15 C, solid precipitation, added cyclohexane solution, maintaining the stirring speed 200-230rpm, filtration, dehydration with dehydrating agent, got white solid2-chloro- 1 -p-tolyl- 1 -propanone. |
