(2-fluorophenyl)methylhydrazine

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

実験手順: Under argon, 100 g (0.613 mol) of the sodium salt of ethyl cyanopyruvate (preparation analogously to Borsche and Manteuffel, Liebigs Ann. 1934, 512, 97) in 2.5 l of dioxane are admixed, with efficient stirring and at room temperature, with 111.75 g (75 ml, 0.98 mol) of trifluoroacetic acid, and the mixture is stirred for 10 min, during which a large proportion of the starting material dissolves. 85.93 g (0.613 mol) of 2-fluorobenzylhydrazine are then added, and the mixture is boiled overnight. After cooling, the precipitated sodium trifluoroacetate crystals are filtered off with suction and washed with dioxane, and the crude solution is reacted further. dissolves the mixture is boiled overnight After cooling the precipitated sodium trifluoroacetate crystals are filtered off with suction washed with dioxane the crude solution is reacted further

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

実験手順: 111.75 g (75 ml, 0.98 mol) of trifluoroacetic acid are added to 100 g (0.613 mol) of sodium salt of ethyl cyanopyruvate (prepared in analogy to Borsche and Manteuffel, Liebigs Ann. 1934, 512, 97) in 2.5 l of dioxane under argon with efficient stirring at room temperature, and the mixture is stirred for 10 minutes during which much of the precursor dissolves. Then 85.93 g (0.613 mol) of 2-fluorobenzylhydrazine are added, and the mixture is heated under reflux overnight. After cooling, the crystals of sodium trifluoroacetate which have separated out are filtered off with suction and washed with dioxane, and the solution is reacted further as it is. the mixture is stirred for 10 minutes during which much of the precursor dissolves the mixture is heated under reflux overnight After cooling the crystals of sodium trifluoroacetate which have separated out are filtered off with suction washed with dioxane the solution is reacted further as it

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

実験手順: 111.75 g (75 ml, 0.98 mol) of trifluoroacetic acid are added to 100 g (0.613 mol) of sodium salt of ethyl cyanopyruvate (prepared in analogy to Borsche and Manteuffel, Liebigs Ann. 1934, 512, 97) in 2.5 l of dioxane under argon with efficient stirring at room temperature, and the mixture is stirred for 10 minutes during which much of the precursor dissolves. Then 85.93 g (0.613 mol) of 2-fluorobenzylhydrazine are added, and the mixture is boiled overnight. After cooling, the crystals of sodium trifluoroacetate which have separated out are filtered off with suction and washed with dioxane, and the solution is reacted further as it is. the mixture is stirred for 10 minutes during which much of the precursor dissolves After cooling the crystals of sodium trifluoroacetate which have separated out are filtered off with suction washed with dioxane the solution is reacted further as it

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

実験手順: 111.75 g (75 ml, 0.98 mol) of trifluoroacetic acid are added to 100 g (0.613 mol) of sodium salt of ethyl cyanopyruvate (prepared in analogy to Borsche and Manteuffel, Liebigs Ann. 1934, 512, 97) in 2.5 l of dioxane under argon with efficient stirring at room temperature, and the mixture is stirred for 10 minutes during which much of the precursor dissolves. Then 85.93 g (0.613 mol) of 2-fluorobenzylhydrazine are added, and the mixture is boiled overnight. After cooling, the crystals of sodium trifluoroacetate which have separated out are filtered off with suction and washed with dioxane, and the solution is reacted further as it is. the mixture is stirred for 10 minutes during which much of the precursor dissolves After cooling the crystals of sodium trifluoroacetate which have separated out are filtered off with suction washed with dioxane the solution is reacted further as it

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

実験手順: 30.2 g of β-amino-β-ethoxyacrylic acid ethyl ester together with 2 g of p-toluenesulphonic acid were dissolved in 300 ml of ethanol and 27.1 g of o-fluorobenzylhydrazine were added under nitrogen. After stirring for two hours, the mixture was left to stand overnight and the compound identified above, which had separated out as a precipitate, was filtered off and recrystallised from ethanol. Melting point: 146°, 11 g (27%). the mixture was left to stand overnight had separated out as a precipitate was filtered off recrystallised from ethanol

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

実験手順: 30.2 g of β-amino-β-ethoxyacrylic acid ethyl ester together with 2 g of p-toluenesulphonic acid were dissolved in 300 ml of ethanol and 27.1 g of o-fluorobenzylhydrazine were added under nitrogen. After stirring for two hours, the mixture was left to stand overnight and the compound identified above, which had separated out as a precipitate, was filtered off and recrystallised from ethanol. Melting point: 146°, 11 g (27%). the mixture was left to stand overnight had separated out as a precipitate was filtered off recrystallised from ethanol

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

実験手順: 30.2 g of β-amino-β-ethoxyacrylic acid ethyl ester together with 2 g of p-toluenesulphonic acid were dissolved in 300 ml of ethanol and 27.1 g of o-fluorobenzylhydrazine were added under nitrogen. After stirring for two hours, the mixture was left to stand overnight and the compound identified above, which had separated out as a precipitate, was filtered off and recrystallised from ethanol. Melting point: 146°, 11 g (27%). the mixture was left to stand overnight had separated out as a precipitate was filtered off recrystallised from ethanol

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

実験手順: Under argon, 100 g (0.613 mol) of the sodium salt of ethyl cyanopyruvate (preparation analogously to Borsche and Manteuffel, Liebigs Ann. 1934, 512, 97) in 2.5 l of dioxane are admixed, with efficient stirring and at room temperature, with 111.75 g (75 ml, 0.98 mol) of trifluoroacetic acid, and the mixture is stirred for 10 min, during which a large proportion of the starting material dissolves. 85.93 g (0.613 mol) of 2-fluorobenzylhydrazine are then added, and the mixture is boiled overnight. After cooling, the precipitated sodium trifluoroacetate crystals are filtered off with suction and washed with dioxane, and the crude solution is reacted further. dissolves the mixture is boiled overnight After cooling the precipitated sodium trifluoroacetate crystals are filtered off with suction washed with dioxane the crude solution is reacted further

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

実験手順: 111.75 g (75 ml, 0.98 mol) of trifluoroacetic acid are added to 100 g (0.613 mol) of sodium salt of ethyl cyanopyruvate (prepared in analogy to Borsche and Manteuffel, Liebigs Ann. 1934, 512, 97) in 2.5 l of dioxane under argon with efficient stirring at room temperature, and the mixture is stirred for 10 minutes during which much of the precursor dissolves. Then 85.93 g (0.613 mol) of 2-fluorobenzylhydrazine are added, and the mixture is heated under reflux overnight. After cooling, the crystals of sodium trifluoroacetate which have separated out are filtered off with suction and washed with dioxane, and the solution is reacted further as it is. the mixture is stirred for 10 minutes during which much of the precursor dissolves the mixture is heated under reflux overnight After cooling the crystals of sodium trifluoroacetate which have separated out are filtered off with suction washed with dioxane the solution is reacted further as it

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

実験手順: 111.75 g (75 ml, 0.98 mol) of trifluoroacetic acid are added to 100 g (0.613 mol) of sodium salt of ethyl cyanopyruvate (prepared in analogy to Borsche and Manteuffel, Liebigs Ann. 1934, 512, 97) in 2.5 l of dioxane under argon with efficient stirring at room temperature, and the mixture is stirred for 10 minutes during which much of the precursor dissolves. Then 85.93 g (0.613 mol) of 2-fluorobenzylhydrazine are added, and the mixture is heated under reflux overnight. After cooling, the crystals of sodium trifluoroacetate which have separated out are filtered off with suction and washed with dioxane, and the solution is reacted further as it is. the mixture is stirred for 10 minutes during which much of the precursor dissolves the mixture is heated under reflux overnight After cooling the crystals of sodium trifluoroacetate which have separated out are filtered off with suction washed with dioxane the solution is reacted further as it

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

実験手順: 111.75 g (75 ml, 0.98 mol) of trifluoroacetic acid are added to 100.00 g (0.613 mol) of the sodium salt of ethyl cyanopyruvate (prepared in analogy to Borsche and Manteuffel, Liebigs Ann. 1934, 512, 97) while stirring efficiently in 2.5 l of dioxane at room temperature under argon, and the mixture is stirred for 10 min, during which most of the precursor dissolves. Then 85.93 g (0.613 mol) of 2-fluorobenzyl-hydrazine are added, and the mixture is boiled overnight. After cooling, the sodium trifluoroacetate crystals which have separated out are filtered off with suction and washed with dioxane, and the remaining crude solution is reacted further. dissolves the mixture is boiled overnight After cooling the sodium trifluoroacetate crystals which have separated out are filtered off with suction washed with dioxane the remaining crude solution is reacted further

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

実験手順: 111.75 g (75 ml, 0.98 mol) of trifluoroacetic acid are added to 100.00 g (0.613 mol) of the sodium salt of ethyl cyanopyruvate (prepared in analogy to Borsche and Manteuffel, Liebigs Ann. 1934, 512, 97) while stirring efficiently in 2.5 l of dioxane at room temperature under argon, and the mixture is stirred for 10 min, during which most of the precursor dissolves. Then 85.93 g (0.613 mol) of 2-fluorobenzyl-hydrazine are added, and the mixture is boiled overnight. After cooling, the sodium trifluoroacetate crystals which have separated out are filtered off with suction and washed with dioxane, and the remaining crude solution is reacted further. dissolves the mixture is boiled overnight After cooling the sodium trifluoroacetate crystals which have separated out are filtered off with suction washed with dioxane the remaining crude solution is reacted further