1-methoxy-2-[2-[2-(2-methoxyethoxy)ethoxy]ethoxy]ethane

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: In using the dioxane solvent of "H", it is preferred to develop first with dioxane alone, followed by a mixture of dioxane and alkanol and finished with alkanol alone (for example, dioxane/dioxane:methanol mixture/methanol).

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

実験手順: In using the dioxane solvent of "H", it is preferred to develop first with dioxane alone, followed by a mixture of dioxane and alkanol and finished with alkanol alone (for example, dioxane/dioxane:methanol mixture/methanol).

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

実験手順: However, in reality, it can be prepared by reacting tetrafluoroethane-β-sultone, KF and CF2═CFCF2OSO2F without isolating FOCCF2SO2F as the intermediate. Specifically, for example, in the presence of a solvent such as tetraglyme, KF and tetrafluoroethane-β-sultone are reacted under cooling, and CF2═CFCF2OSO2F is dropwise added thereto and reacted, whereby CF2═CFCF2OCF2CF2SO2F can be obtained. However, in reality, it can be prepared without isolating FOCCF2SO2F as the intermediate under cooling reacted

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

実験手順: However, in reality, it can be prepared by reacting tetrafluoroethane-β-sultone, KF and CF2═CFCF2OSO2F without isolating FOCCF2SO2F as the intermediate. Specifically, for example, in the presence of a solvent such as tetraglyme, KF and tetrafluoroethane-β-sultone are reacted under cooling, and CF2═CFCF2OSO2F is dropwise added thereto and reacted, whereby CF2═CFCF2OCF2CF2SO2F can be obtained. However, in reality, it can be prepared without isolating FOCCF2SO2F as the intermediate under cooling reacted

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

実験手順: In using the dioxane solvent of "H", it is preferred to develop first with dioxane alone, followed by a mixture of dioxane and alkanol and finished with alkanol alone (for example, dioxane/dioxane:methanol mixture/methanol).

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

実験手順: In using the dioxane solvent of "H", it is preferred to develop first with dioxane alone, followed by a mixture of dioxane and alkanol and finished with alkanol alone (for example, dioxane/dioxane:methanol mixture/methanol).

反応条件: temp:47.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Sodium borohydride (0.32 g) was added to 25 g tetraglyme with rapid stirring. At room temperature 4.8 g of Cut 2 (b.p. 110°-130° C.) from Example 11, F5S(CF2)3CO2CH3, was added to the sodium borohydride solution over a period of 1.5 hrs. The crude reaction mixture was heated to 47° C. and held at that temperature for one hr. The reaction mixture then was cooled to room temperature and 50 mL water was added. After the water was added, 1 mL of concentrated sulfuric acid was introduced. The reaction mixture was heated to 100° C., at which point an azeotrope of the fluorochemical and water distilled from the reaction mixture. The crude reaction mixture was heated until no more fluorochemical distillate was produced. The water and fluorochemical were phase-separated. A total of 2.2 g crude fluorochemical, a yellow foul-smelling liquid, was collected. GC-mass spectral, IR, and F19 nmr spectral analyses showed the liquid to comprise following composition (in mole %): 90.9% F5S(CF2)3CH2OH, 1.5% F5SCF(CF3)CF2CH2OH, 0.4% F5SCF2CF(CF3)CH2OH, 3.3% F5S(CF2)3CH(OH)2, 3.8% F5S(CF2)3CH(OH)(CH3) or F5S(CF2)3CH(OH)(CH2Rf). The crude reaction mixture The reaction mixture then was cooled to room temperature distilled from the reaction mixture The crude reaction mixture was heated until no more fluorochemical distillate was produced The water and fluorochemical were phase-separated A total of 2.2 g crude fluorochemical, a yellow foul-smelling liquid, was collected