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0 °C

To a solution wherein 6-amino-5-chloro-1,1,3,3-tetrafluoro-1,3-dihydroisobenzofuran (2.41 g, 10.0 mmol) is in acetic acid (30 ml), a nitrosylsulfuric acid solution prepared from sodium nitrite (760 mg, 11.0 mmol) and concentrated sulfuric acid (5.5 ml) was added dropwise at 10 to 15° C. over a period of about 10 minutes. The reaction solution was then added dropwise into a solution consisting of stannous chloride anhydride (9.5 g) and concentrated hydrochloric acid (8 ml) under vigorous stirring at 0° C. and further stirred for 30 minutes. After a sodium hydroxide solution was added to the reaction mixture to make the solution alkaline, the solution was extracted with diethyl ether, and the organic layer was then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure and the residue was subjected to silica gel column chromatography to give 1.8 g of 5-chloro-1,1,3,3-tetrafluoro-1,3-dihydroisobenzofuran-6-yl-hydrazine.

1. additionwas added dropwise at 10 to 15° C. over a period of about 10 minutes
2. additionThe reaction solution was then added dropwise into a solution
3. stirringfurther stirred for 30 minutes
4. extractionthe solution was extracted with diethyl ether
5. dry with materialthe organic layer was then dried over anhydrous magnesium sulfate
6. distillationThe solvent was distilled off under reduced pressure