Hydrazine, [(4-fluorophenyl)Methyl]-, hydrochloride (1:2)

反応条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of (4-fluorobenzyl)hydrazine dihydrochloride (1.0 g, 4.7 mmol, Matrix) in ethyl alcohol (2 mL) was added 4,4-dimethyl-3-oxopentanenitrile (0.6 g, 4.7 mmol, Aldrich). After stirring at 85° C. for 2 h, the reaction mixture was cooled, concentrated, diluted with ethyl acetate (10 mL) and washed with saturated NaHCO3 (10 mL). The aqueous layer was extracted with ethyl acetate (2×10 mL). The combined organic extracts were dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to obtain 1.3 g (99%) of the title compound. MS (ESI+) m/z 248 (M+H)+. the reaction mixture was cooled concentrated diluted with ethyl acetate (10 mL) washed with saturated NaHCO3 (10 mL) The aqueous layer was extracted with ethyl acetate (2×10 mL) The combined organic extracts were dried over anhydrous Na2SO4 filtered concentrated under reduced pressure

反応条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of (4-fluorobenzyl)hydrazine dihydrochloride (1.0 g, 4.7 mmol, Matrix) in ethyl alcohol (2 mL) was added 4,4-dimethyl-3-oxopentanenitrile (0.6 g, 4.7 mmol, Aldrich). After stirring at 85° C. for 2 h, the reaction mixture was cooled, concentrated, diluted with ethyl acetate (10 mL) and washed with saturated NaHCO3 (10 mL). The aqueous layer was extracted with ethyl acetate (2×10 mL). The combined organic extracts were dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to obtain 1.3 g (99%) of the title compound. MS (ESI+) m/z 248 (M+H)+. the reaction mixture was cooled concentrated diluted with ethyl acetate (10 mL) washed with saturated NaHCO3 (10 mL) The aqueous layer was extracted with ethyl acetate (2×10 mL) The combined organic extracts were dried over anhydrous Na2SO4 filtered concentrated under reduced pressure

反応条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of (4-fluorobenzyl)hydrazine dihydrochloride (1.0 g, 4.7 mmol, Matrix) in ethyl alcohol (2 mL) was added 4,4-dimethyl-3-oxopentanenitrile (0.6 g, 4.7 mmol, Aldrich). After stirring at 85° C. for 2 h, the reaction mixture was cooled, concentrated, diluted with ethyl acetate (10 mL) and washed with saturated NaHCO3 (10 mL). The aqueous layer was extracted with ethyl acetate (2×10 mL). The combined organic extracts were dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to obtain 1.3 g (99%) of the title compound. MS (ESI m/z 248 (M+H)+. the reaction mixture was cooled concentrated diluted with ethyl acetate (10 mL) washed with saturated NaHCO3 (10 mL) The aqueous layer was extracted with ethyl acetate (2×10 mL) The combined organic extracts were dried over anhydrous Na2SO4 filtered concentrated under reduced pressure

反応条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of (4-fluorobenzyl)hydrazine dihydrochloride (1.0 g, 4.7 mmol, Matrix) in ethyl alcohol (2 mL) was added 4,4-dimethyl-3-oxopentanenitrile (0.6 g, 4.7 mmol, Aldrich). After stirring at 85° C. for 2 h, the reaction mixture was cooled, concentrated, diluted with ethyl acetate (10 mL) and washed with saturated NaHCO3 (10 mL). The aqueous layer was extracted with ethyl acetate (2×10 mL). The combined organic extracts were dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to obtain 1.3 g (99%) of the title compound. MS (ESI+) m/z 248 (M+H)+. the reaction mixture was cooled concentrated diluted with ethyl acetate (10 mL) washed with saturated NaHCO3 (10 mL) The aqueous layer was extracted with ethyl acetate (2×10 mL) The combined organic extracts were dried over anhydrous Na2SO4 filtered concentrated under reduced pressure