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PREPARATION 14 N-(4-Fluoro-2-methylphenyl)acetamide In the manner of Preparation 5, 20 g (0.160 mol) of 5-fluoro-2-methylaniline was converted into the title compound: yield 25.0 g (94%); m.p. 131-132 C., [lit. m.p. 133.5-134 C.: E. A. Steck, L. T. Fletcher, J. Am. Chem. Soc. 70, 439-440 (1948)].
With calcium carbonate; In hydrogenchloride; dichloromethane; water;
(Step 6) Synthesis of 5-fluoro-2-methylphenyl isothiocyanate Under stirring at 0?C, a solution of 5-fluoro-2-methylaniline (1.23 g, 9.84 mmol) in methylene chloride (10 ml) was added dropwise to a mixture of calcium carbonate (2.46 g, 24.6 mmol) and thiophosgene (750 ?l, 9.84 mmol) in a methylene chloride/water (1/1, 40 ml) mixture. After completion of the dropwise addition, the reaction mixture was stirred further at 0?C for 35 minutes. The reaction mixture was poured in ice-1N HCl, followed by extraction with chloroform. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, and distilled under reduced pressure to remove the solvent to give 5-fluoro-2-methylphenyl isothiocyanate (1.45 g, 88%) as a brown oil. MS (ESI) m/z 167 (M+).
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