Methyl perfluoroheptanoate

Conditions: temp:45.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A 3-1, four-necked, round-bottomed flask equipped with stirrer, thermometer, reflux condenser with bubble counter and inlet gas-tube, is charged with 658 g (1.74 mol) of methyl perfluoroheptanoate and 1.5 l tetrahydrofurane. A stream of ammonia is passed from a pressure tank into the stirring solution. The ammonia feed rate is such that a negligible amount of gas is observed exiting the reactor as observed in the bubble counter. Temperature of the mixture increases to 40-50° C. Ammonium supply is continued until the temperature begins to decrease and an increasing volume of gas is observed exiting the reactor in the bubble counter. After ending the ammonia supply, the mixture is left to stand for 12 hr. Solvent is removed under reduced pressure, yielding 626 g p perfluoroheptanoic acid amide (99%), mp 127-128° C. A 3-1, four-necked, round-bottomed flask equipped with stirrer thermometer, reflux condenser with bubble counter and inlet gas-tube the mixture is left Solvent is removed under reduced pressure

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A 2-1, four-necked, round-bottomed flask equipped with stirrer, addition funnel, thermometer and reflux condenser, is charged with 728 g (2 mol) of dried perfluoroheptanoic acid, 160 g (5 mol) of methanol. The mixture is stirred and added dropwise 50 ml concentrated sulfuric acid and then heated to reflux for 4 hr. At the end of the reflux period the mixture is cooled to room temperature and poured into 2 l cold water. After separation of the phases, the lower organic phase is washed with water till pH neutral and dried over CaCl2. Distillation of the crude gives 658 g (87%) of methyl perfluoroheptanoate, bp 139° C. A 2-1, four-necked, round-bottomed flask equipped with stirrer, addition funnel thermometer and reflux condenser heated to reflux for 4 hr After separation of the phases the lower organic phase is washed with water till pH neutral and dried over CaCl2 Distillation of the crude