2-hydrazinylethanol

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 1-Fluoro-4-nitrobenzene (7.1 g, 50 mmol) was dissolved in CH3CN (70 ml), 2-hydroxyethylhyrazine (purity: 90%, Aldrich, 5.0 g, 66 mmol) and K2CO3 (7.6 g, 55 mmol) were added thereto. The suspension thus obtained was stirred for 4 hrs with reflux. The resulting orange-colored suspension was concentrated under reduced pressure (reflux condenser, 10 torr, 40° C.) and ethylacetate (EA, 90 ml) and water (18 ml) were added thereto. The resulting mixture was stirred strongly at r.t. for 10 min. The organic layer was extracted and washed with the saturated brine (10 ml). The resulting solution was cooled to 10° C. and 48% HBr solution (3.7 ml) was added thereto dropwise with stirring. The pale yellow colored solid thus obtained was filtered off and dried under high vacuum (1 torr, 40° C.) to obtain the title compound as an intermediate. The suspension thus obtained with reflux The resulting orange-colored suspension was concentrated under reduced pressure (reflux condenser, 10 torr, 40° C.) and ethylacetate (EA, 90 ml) and water (18 ml) were added The resulting mixture was stirred strongly at r.t. for 10 min The organic layer was extracted washed with the saturated brine (10 ml) 48% HBr solution (3.7 ml) was added dropwise with stirring The pale yellow colored solid thus obtained was filtered off dried under high vacuum (1 torr, 40° C.)

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a stirred solution of 3-(7-Methoxy-6-methyl-indan-4-ylmethyl)-pentane-2,4-dione (1.0 gm 0.0036 mole) in Ethanol (15 ml), a solution of 2-Hydrazino-ethanol (0.33 gm, 0.0043 mole) in Ethanol (5 ml) was added at 25-30° C. and reaction mixture was heated to 70° C. for an hour. The Acetic acid (2 ml) was added. Further the reaction mixture was stirred at 70° C. for 3 hours. Ethanol was distilled under vacuum to give a residue which was partitioned between Ethyl acetate (50 ml) and water (25 ml). Ethyl acetate was distilled under vacuum to give a crude product The crude product was solidified after stirring in Diethyl ether (10 ml). The solid was filtered under vacuum and dried to give a 700 mg of desired compound as a solid. reaction mixture Ethanol was distilled under vacuum to give a residue which was partitioned between Ethyl acetate (50 ml) and water (25 ml) Ethyl acetate was distilled under vacuum to give a crude product The crude product The solid was filtered under vacuum dried

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

実験手順: A mixture of 5.0 g. of 6-(p-chlorophenyl)-3-chloropyridazine and 5.02 g. of 2-hydroxyethylhydrazine in 75 ml. of butanol is heated at reflux overnight and then cooled in an ice bath. The precipitate is collected by filtration, washed with butanol, water and then dried. Recrystallization from ethanol gives crystals, m.p. 172°-174° C. A mixture of 5.0 g at reflux overnight cooled in an ice bath The precipitate is collected by filtration washed with butanol, water dried Recrystallization from ethanol gives crystals, m.p. 172°-174° C.

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

実験手順: A solution of 2-(2-fluorophenyl)-3-hydroxy-4-methyl-5-(3-methoxyphenyl)-2,4-cyclopentadienone (620 mg, 2 mmol) and hydroxylethylhydrazine (360 mg, 45 mmol)) in ethanol (5 mL) was heated at reflux for 6 hours. The resulting solution was concentrated in vacuo and the residue was dissolved in ethyl acetate (80 mL), washed with brine, dried over magnesium sulfate, filtered and concentrated in vacuo to give the desired compound as colorless oil. MS: 369 (MH+). at reflux for 6 hours The resulting solution was concentrated in vacuo the residue was dissolved in ethyl acetate (80 mL) washed with brine dried over magnesium sulfate filtered concentrated in vacuo

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir: