反应详情

Cyclopropyl(2-fluoro-4-hydroxyphenyl)methanone (6.51 g) which can be prepared according to the method described in Reference example 2, etc., sodium acetate (14.3163 g; manufactured by Wako Pure Chemical Industries, Ltd.), and benzylhydrazine-dihydrochloride (10.72 g; manufactured by Sigma-Aldrich Co.) were suspended in xylene (180 mL). By using a dean-stark apparatus, the mixture was stirred overnight at reflux. After cooling to room temperature, the mixture was added with water and extracted twice with ethyl acetate. The organic layer was washed twice with water and brine and dried over anhydrous sodium sulfate. After the solvent was evaporated under reduced pressure, insoluble matters were dissolved by adding n-hexane to the residue and the title compound was obtained as a crude product (10.97 g).

1. temperatureat reflux
2. extractionextracted twice with ethyl acetate
3. washThe organic layer was washed twice with water and brine
4. dry with materialdried over anhydrous sodium sulfate
5. customAfter the solvent was evaporated under reduced pressure, insoluble matters
6. dissolutionwere dissolved
7. additionby adding n-hexane to the residue