3-全氟己基丙醇

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

实验步骤: 2-iodo-4,4,5,5,6,6,7,7,8,8,9,9,9-tridecafluorononan-1-ol 19 (15 g, 29.8 mmol) was slowly added to a solution of lithium aluminum hydride (1.14 g, 30.1 mmol) in THF (60 mL). After stirring at room temperature overnight, the reaction mixture was quenched with ethylacetate (5 mL). Water (150 mL) was added to the mixture and extracted with ether (3×75 mL). Ether layers were combined, washed with water and brine solution. The ether layer was then concentrated and distilled to get 20 (8.66 g, 77%) bp 90-92° C. at aspirator pressure; 1H NMR (CDCl3) δ3.75 (t, J=6.1 Hz, 2H), δ2.31-2.13 (mn, 2H), δ1.92-1.83 (mn, 2H) the reaction mixture was quenched with ethylacetate (5 mL) Water (150 mL) was added to the mixture extracted with ether (3×75 mL) washed with water and brine solution The ether layer was then concentrated distilled

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

实验步骤: 2-iodo-4,4,5,5,6,6,7,7,8,8,9,9,9-tridecafluorononan-1-ol 19 (15 g, 29.8 mmol) was slowly added to a solution of lithium aluminum hydride (1.14 g, 30.1 mmol) in THF (60 mL). After stirring at room temperature overnight, the reaction mixture was quenched with ethylacetate (5 mL). Water (150 mL) was added to the mixture and extracted with ether (3×75 mL). Ether layers were combined, washed with water and brine solution. The ether layer was then concentrated and distilled to get 20 (8.66 g, 77%) bp 90-92° C. at aspirator pressure; 1H NMR (CDCl3) δ3.75 (t, J=6.1 Hz, 2H), δ2.31-2.13 (mn, 2H), δ1.92-1.83 (mn, 2H) the reaction mixture was quenched with ethylacetate (5 mL) Water (150 mL) was added to the mixture extracted with ether (3×75 mL) washed with water and brine solution The ether layer was then concentrated distilled

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

实验步骤: After confirming disappearance of C6F13CH═CH2 by gas chromatography, the reaction was terminated by cooling to obtain a reaction liquid. From the obtained reaction liquid, majority of methanol was distilled off under reduced pressure, and then, the reaction liquid was washed with water to remove the remaining methanol thereby to obtain 430 g of C6F13CH2CH2CH2OH having a purity of 92.8%. the reaction was terminated by cooling to obtain a reaction liquid was distilled off under reduced pressure the reaction liquid was washed with water to remove the remaining methanol

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

实验步骤: 2-iodo-4,4,5,5,6,6,7,7,8,8,9,9,9-tridecafluorononan-1-ol 19 (15 g, 29.8 mmol) was slowly added to a solution of lithium aluminum hydride (1.14 g, 30.1 mmol) in THF (60 mL). After stirring at room temperature overnight, the reaction mixture was quenched with ethylacetate (5 mL). Water (150 mL) was added to the mixture and extracted with ether (3×75 mL). Ether layers were combined, washed with water and brine solution. The ether layer was then concentrated and distilled to get 20 (8.66 g, 77%) bp 90-92° C. at aspirator pressure; 1H NMR (CDCl3) δ3.75 (t, J=6.1 Hz, 2H), δ2.31-2.13 (mn, 2H), δ1.92-1.83 (mn, 2H) the reaction mixture was quenched with ethylacetate (5 mL) Water (150 mL) was added to the mixture extracted with ether (3×75 mL) washed with water and brine solution The ether layer was then concentrated distilled