三乙酰甲烷

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Gaseous acetyl fluoride is bubbled into a suspension of 30.0 g. (0.1 mole) of the thallous salt of acetylacetone in 150 ml. of dry tetrahydrofuran, under nitrogen, at a rate of 3.0 cc./minute for a total of 30 minutes. After filtration through Celite, the solution is concentrated and the residue distilled to give 13.5 g. (96%), b.p. 90°-95°/1.0 mm. Gaseous acetyl fluoride is bubbled into a suspension of 30.0 g for a total of 30 minutes After filtration through Celite the solution is concentrated the residue distilled to give 13.5 g

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Gaseous acetyl fluoride is bubbled into a suspension of 30.0 g. (0.1 mole) of the thallous salt of acetylacetone in 150 ml. of dry tetrahydrofuran, under nitrogen, at a rate of 3.0 cc./minute for a total of 30 minutes. After filtration through Celite, the solution is concentrated and the residue distilled to give 13.5 g. (96%), b.p. 90°-95°/1.0 mm. Gaseous acetyl fluoride is bubbled into a suspension of 30.0 g for a total of 30 minutes After filtration through Celite the solution is concentrated the residue distilled to give 13.5 g

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Gaseous acetyl fluoride is bubbled into a suspension of 30.0 g. (0.1 mole) of the thallous salt of acetylacetone in 150 ml. of dry tetrahydrofuran, under nitrogen, at a rate of 3.0 cc./minute for a total of 30 minutes. After filtration through Celite, the solution is concentrated and the residue distilled to give 13.5 g. (96%), b.p. 90°-95°/1.0 mm. Gaseous acetyl fluoride is bubbled into a suspension of 30.0 g for a total of 30 minutes After filtration through Celite the solution is concentrated the residue distilled to give 13.5 g

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Gaseous acetyl fluoride is bubbled into a suspension of 30.0 g. (0.1 mole) of the thallous salt of acetylacetone in 150 ml. of dry tetrahydrofuran, under nitrogen, at a rate of 3.0 cc./minute for a total of 30 minutes. After filtration through Celite, the solution is concentrated and the residue distilled to give 13.5 g. (96%), b.p. 90°-95°/1.0 mm. Gaseous acetyl fluoride is bubbled into a suspension of 30.0 g for a total of 30 minutes After filtration through Celite the solution is concentrated the residue distilled to give 13.5 g

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Gaseous acetyl fluoride is bubbled into a suspension of 30.0 g. (0.1 mole) of the thallous salt of acetylacetone in 150 ml. of dry tetrahydrofuran, under nitrogen, at a rate of 3.0 cc./minute for a total of 30 minutes. After filtration through Celite, the solution is concentrated and the residue distilled to give 13.5 g. (96%), b.p. 90°-95°/1.0 mm. Gaseous acetyl fluoride is bubbled into a suspension of 30.0 g for a total of 30 minutes After filtration through Celite the solution is concentrated the residue distilled to give 13.5 g

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Gaseous acetyl fluoride is bubbled into a suspension of 30.0 g. (0.1 mole) of the thallous salt of acetylacetone in 150 ml. of dry tetrahydrofuran, under nitrogen, at a rate of 3.0 cc./minute for a total of 30 minutes. After filtration through Celite, the solution is concentrated and the residue distilled to give 13.5 g. (96%), b.p. 90°-95°/1.0 mm. Gaseous acetyl fluoride is bubbled into a suspension of 30.0 g for a total of 30 minutes After filtration through Celite the solution is concentrated the residue distilled to give 13.5 g

反应条件: temp:-10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 1.86 g of aminoguanidine hydrochloride were added to a solution of 3.0 g of triacetylmethane and 30 ml of methanol with cooling at -10° C., and the reaction mixture was stirred for one day with cooling with ice. The solvent was removed by distillation under reduced pressure, and the resulting residue was purified by silica gel chromatography (eluent: chloroform/methanol=5/1) and then recrystallized from ether-chloroform to obtain 484 mg of 4-acetyl-3,5-dimethyl-1H-pyrazole-1-carboxamidine. with cooling with ice The solvent was removed by distillation under reduced pressure the resulting residue was purified by silica gel chromatography (eluent: chloroform/methanol=5/1) recrystallized from ether-chloroform

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Gaseous acetyl fluoride is bubbled into a suspension of 30.0 g. (0.1 mole) of the thallous salt of acetylacetone in 150 ml. of dry tetrahydrofuran, under nitrogen, at a rate of 3.0 cc./minute for a total of 30 minutes. After filtration through Celite, the solution is concentrated and the residue distilled to give 13.5 g. (96%), b.p. 90°-95°/1.0 mm. Gaseous acetyl fluoride is bubbled into a suspension of 30.0 g for a total of 30 minutes After filtration through Celite the solution is concentrated the residue distilled to give 13.5 g

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Gaseous acetyl fluoride is bubbled into a suspension of 30.0 g. (0.1 mole) of the thallous salt of acetylacetone in 150 ml. of dry tetrahydrofuran, under nitrogen, at a rate of 3.0 cc./minute for a total of 30 minutes. After filtration through Celite, the solution is concentrated and the residue distilled to give 13.5 g. (96%), b.p. 90°-95°/1.0 mm. Gaseous acetyl fluoride is bubbled into a suspension of 30.0 g for a total of 30 minutes After filtration through Celite the solution is concentrated the residue distilled to give 13.5 g