1,1,1,2,2,3,3-Heptafluoro-5-iodopentane

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: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:; See reaction.notes.procedure_details.

実験手順: 3.55 g of methylamine is condensed in a solution of 2.6 ml of 1,1,1,2,2,3,3 heptafluor-5-iodo-pentane in 20 ml of anhydrous tetrahydrofuran at −40° C., and it is stirred overnight at room temperature in a pressurized reactor. After the pressurized reactor was opened at −30° C., it is allowed to come to room temperature to allow excess methylamine to evaporate off. Then, the reaction solution is mixed with diethyl ether, washed with saturated common salt solution, dried on magnesium sulfate and concentrated by evaporation in a vacuum. 1.26 g of (3,4,4,5,5,5-hexafluoro-pent-2-enyl)-methyl-amine is obtained as a crude product. was opened at −30° C. to come to room temperature to evaporate off Then, the reaction solution is mixed with diethyl ether washed with saturated common salt solution dried on magnesium sulfate concentrated by evaporation in a vacuum

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

実験手順: In 50 ml of acetone, 3.2 g of 2-(2,2,3,3,3-pentafluoropropyl)malononitrile and 7.2 g of 5-iodo-1,1,1,2,2,3,3-heptafluoropentane were dissolved, 3.2 g of potassium carbonate was added and the mixture was stirred at room temperature for 10 hours. Thereafter, dilute hydrochloric acid was added to the reaction mixture and the mixture was extracted with t-butyl methyl ether. The organic layer was washed successively with water, aqueous saturated sodium hydrogen carbonate and aqueous saturated sodium chloride, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.05 g of 2-(3,3,4,4,5,5,5-heptafluoropentyl)-2-(2,2,3,3,3-pentafluoropropyl)malononitrile (hereinafter, referred to as the present compound (96)): the mixture was extracted with t-butyl methyl ether The organic layer was washed successively with water, aqueous saturated sodium hydrogen carbonate and aqueous saturated sodium chloride dried over anhydrous magnesium sulfate concentrated under reduced pressure

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

実験手順: 1.4 g of 2-(2,2,3,3,4,4,5,5-octafluoropentyl)malononitrile and 1.6 g of 1-iodo-3,3,4,4,5,5,5-heptafluoropentane were dissolved in 5 ml of ethylene glycol dimethyl ether, 0.83 g of potassium carbonate was added, and the mixture was stirred at room temperature for 8 hours. Thereafter, dilute hydrochloric acid was added to the reaction mixture, followed by extraction with methyl tert-butyl ether. The organic layer was washed successively with water, aqueous saturated sodium hydrogen carbonate and aqueous saturated sodium chloride, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.75 g of 2-(3,3,4,4,5,5,5-heptafluoropentyl)-2-(2,2,3,3,4,4,5,5-octafluoropentyl)malononitrile (hereinafter, referred to as the present compound (71)). followed by extraction with methyl tert-butyl ether The organic layer was washed successively with water, aqueous saturated sodium hydrogen carbonate and aqueous saturated sodium chloride dried over anhydrous magnesium sulfate concentrated under reduced pressure