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With caesium carbonate In N,N-dimethyl-formamide at 20 - 23℃;
EXAMPLES Preparation 1Methyl 4-chloro-3-methylbenzoateTo a solution of 4~chloro-3-methylbenzoic acid (25 g) in DMF (550 ml) under a dry atmosphere was added portion wise 50 g of caesium carbonate and then slowly, 10,95 ml of methyl iodide. Temperature rose from 200C to 23 0C. The reaction mixture was stirred at room temperature overnight. The mixture was cooled to 10 0C and then 800 ml of an aqueous solution of NaHCO3 (2percent) and 600 ml of ethyl acetate were successively added. The aqueous layer was separated, extracted again with 400 ml of ethyl acetate. The .bul. combined organic layers were washed successively with 2x250 ml of an aqueous solution of NaHCO3 (2percent), then 2x250 ml of aqueous solution of NaCl (2percent), dried over Na2SO4 and concentrated in vacuum. The residue was purified by distillation to afford 25.31 g of a clear yellow liquid (b.p.: 78 °C/0.08 mbar). Yield: 93percentT.L.C.: Silica gel, eluents: cyclohexane-ethyl acetate 75/25
4-chloro-3-methyl benzoic acid 5.2 g (0.03 mol), CH3OH 40 mLand H2SO4 1 mL were refluxed for 8 h. After completion of the reaction as indicated by TLC. The solvent was evaporated under reduced pressure and the residue was dissolved in ethyl acetate 100 mL. Then the liquid was washed with saturated Na2CO3, waterand saturated NaCl successively. The organic layer was dried over anhydrous Na2SO4 and concentrated. The residue was dried to afford X13 5.1 g (90.1 percent), mp: 76-78 °C.
Reference：
[1] European Journal of Medicinal Chemistry, 2015, vol. 90, p. 170 - 183
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[ 1044920-98-0 ]
Reference：
[1] European Journal of Medicinal Chemistry, 2015, vol. 90, p. 170 - 183
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