1,6-己二醇

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

实验步骤: Furoyl chloride 121 g (0.93 m) added to 52 g (0.44 m) hexanediol, 133 g (1.3 m) triethylamine and 485 g methylene chloride at 5°-10°. Yield of 92 g recrystallized from isopropyl alchol, 69°-71° m.p. Yield of 92 g recrystallized from isopropyl alchol, 69°-71° m.p.

反应条件: temp:185.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a fashion similar to Example 8, hexanediol was alkylated with n-octyl bromide, the product was acetylated, and the resulting C8H17—O—(CH2)6—O—COCH3 was directly fluorinated and hydrolyzed as in Example 8 to C8F17—O—(CF2)5COOH, which was recrystallized from perfluorohexane. The recrystallized acid (37.5 g) was mixed with 4.0 g NaOH and 100 mL ethylene glycol and heated to 185° C. The product was washed with water, and the residual 27.9 g was distilled to give pure C8F17—O—(CF2)5H, micro b.p. 195° C. was recrystallized from perfluorohexane The recrystallized acid (37.5 g) was mixed with 4.0 g NaOH and 100 mL ethylene glycol The product was washed with water the residual 27.9 g was distilled

反应条件: temp:185.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a fashion similar to Example 8, hexanediol was alkylated with n-octyl bromide, the product was acetylated, and the resulting C8H17—O—(CH2)6—O—COCH3 was directly fluorinated and hydrolyzed as in Example 8 to C8F17—O—(CF2)5COOH, which was recrystallized from perfluorohexane. The recrystallized acid (37.5 g) was mixed with 4.0 g NaOH and 100 mL ethylene glycol and heated to 185° C. The product was washed with water, and the residual 27.9 g was distilled to give pure C8F17—O—(CF2)5H, micro b.p. 195° C. was recrystallized from perfluorohexane The recrystallized acid (37.5 g) was mixed with 4.0 g NaOH and 100 mL ethylene glycol The product was washed with water the residual 27.9 g was distilled

反应条件: temp:185.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a fashion similar to Example 8, hexanediol was alkylated with n-octyl bromide, the product was acetylated, and the resulting C8H17—O—(CH2)6—O—COCH3 was directly fluorinated and hydrolyzed as in Example 8 to C8F17—O—(CF2)5COOH, which was recrystallized from perfluorohexane. The recrystallized acid (37.5 g) was mixed with 4.0 g NaOH and 100 mL ethylene glycol and heated to 185° C. The product was washed with water, and the residual 27.9 g was distilled to give pure C8F17—O—(CF2)5H, micro b.p. 195° C. was recrystallized from perfluorohexane The recrystallized acid (37.5 g) was mixed with 4.0 g NaOH and 100 mL ethylene glycol The product was washed with water the residual 27.9 g was distilled

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

实验步骤: 661.9 g of the ethylene oxide polyether started from trimethylolpropane esterified with 2 mol acrylic acid (12 mol ethylene oxide per mol trimethylolpropane) and 164.4 g of a polyester polyol from hexanediol and adipic acid (OH number 314, equivalent weight 178.5 g), 1.0 g 2,6-di-tert-butyl-4-methyl-phenol and 1.0 g tin octoate were initially introduced into the reaction vessel. 148.8 g Desmodur® T80 (toluylene diisocyanate, commercial product of Bayer AG, Leverkusen) were metered in at 50 to 60° C. After a further 5 h 31.6 g isophorone-diisocyanate were metered in. The reaction was carried out at 60° C. for a further 5 h and 74.0 g of the ethylene oxide polyether started from trimethylolpropane esterified with 2 mol acrylic acid (12 mol ethylene oxide per mol trimethylolpropane) were then added. The reaction was subsequently carried out at 60° C. until the NCO content of the solution was less than 0.10 wt. %. were initially introduced into the reaction vessel were metered in at 50 to 60° C were then added

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

实验步骤: 661.9 g of the ethylene oxide polyether started from trimethylolpropane esterified with 2 mol acrylic acid (12 mol ethylene oxide per mol trimethylolpropane) and 164.4 g of a polyester polyol from hexanediol and adipic acid (OH number 314, equivalent weight 178.5 g), 1.0 g 2,6-di-tert-butyl-4-methyl-phenol and 1.0 g tin octoate were initially introduced into the reaction vessel. 148.8 g Desmodur® T80 (toluylene diisocyanate, commercial product of Bayer AG, Leverkusen) were metered in at 50 to 60° C. After a further 5 h 31.6 g isophorone-diisocyanate were metered in. The reaction was carried out at 60° C. for a further 5 h and 74.0 g of the ethylene oxide polyether started from trimethylolpropane esterified with 2 mol acrylic acid (12 mol ethylene oxide per mol trimethylolpropane) were then added. The reaction was subsequently carried out at 60° C. until the NCO content of the solution was less than 0.10 wt. %. were initially introduced into the reaction vessel were metered in at 50 to 60° C were then added

反应条件: temp:185.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a fashion similar to Example 8, hexanediol was alkylated with n-octyl bromide, the product was acetylated, and the resulting C8H17—O—(CH2)6—O—COCH3 was directly fluorinated and hydrolyzed as in Example 8 to C8F17—O—(CF2)5COOH, which was recrystallized from perfluorohexane. The recrystallized acid (37.5 g) was mixed with 4.0 g NaOH and 100 mL ethylene glycol and heated to 185° C. The product was washed with water, and the residual 27.9 g was distilled to give pure C8F17—O—(CF2)5H, micro b.p. 195° C. was recrystallized from perfluorohexane The recrystallized acid (37.5 g) was mixed with 4.0 g NaOH and 100 mL ethylene glycol The product was washed with water the residual 27.9 g was distilled

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

实验步骤: First, dimethyl terephthalate and 1,4-butanediol (the latter in an excess of 5-60, preferably 10-45, mol are reacted with one another at from 150° to 220° C. at from 0.7 to 1.5 bar for from 30 to 90, preferably from 40 to 70, minutes, transesterification taking place and the methanol formed, together with excess butanediol and small amounts of oligomeric and polymeric compounds and residual amounts of dimethyl terephthalate, being transferred with the vapors to a column into which a liquid residue containing dihydroxy compounds, as obtained, for example, in the distillation of 1,4-butanediol or 1,6-hexanediol, is simultaneously introduced. The composition of the residue is not subject per se to any particular restriction, provided that it is in liquid form and no compounds which interfere with the separation in the column are present. This is generally the case for the residues described, which are obtained from the distillation of butanediol and hexanediol. is simultaneously introduced provided that it no compounds which interfere with the separation in the column

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

实验步骤: Pure potassium t-butoxide (50 mmoles, 5.61 g) is added portionwise to a stirred solution of 100 mmoles of hexanediol (11.82 gr) dissolved in 30 ml of THF at room temperature under argon. When addition is complete, 50 mmoles of benzylbromide (5.9 ml) are introduced and the reaction mixture is stirred at room temperature overnight. The white solid is then removed by filtration, the filtrate is evaporated and the residue is dissolved in ethylacetate, washed with saturated ammonium chloride, H2O and brine. Usual workup and purification by flash chromatography gives finally 7.51 g of product (72%). When addition The white solid is then removed by filtration the filtrate is evaporated the residue is dissolved in ethylacetate washed with saturated ammonium chloride, H2O and brine Usual workup and purification by flash chromatography

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

实验步骤: Pure potassium t-butoxide (50 mmoles, 5.61 g) is added portionwise to a stirred solution of 100 mmoles of hexanediol (11.82 gr) dissolved in 30 ml of THF at room temperature under argon. When addition is complete, 50 mmoles of benzylbromide (5.9 ml) are introduced and the reaction mixture is stirred at room temperature overnight. The white solid is then removed by filtration, the filtrate is evaporated and the residue is dissolved in ethylacetate, washed with saturated ammonium chloride, H2O and brine. Usual workup and purification by flash chromatography gives finally 7.51 g of product (72%). When addition The white solid is then removed by filtration the filtrate is evaporated the residue is dissolved in ethylacetate washed with saturated ammonium chloride, H2O and brine Usual workup and purification by flash chromatography

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

实验步骤: Furoyl chloride 121 g (0.93 m) added to 52 g (0.44 m) hexanediol, 133 g (1.3 m) triethylamine and 485 g methylene chloride at 5°-10°. Yield of 92 g recrystallized from isopropyl alchol, 69°-71° m.p. Yield of 92 g recrystallized from isopropyl alchol, 69°-71° m.p.

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

实验步骤: Furoyl chloride 121 g (0.93 m) added to 52 g (0.44 m) hexanediol, 133 g (1.3 m) triethylamine and 485 g methylene chloride at 5°-10°. Yield of 92 g recrystallized from isopropyl alchol, 69°-71° m.p. Yield of 92 g recrystallized from isopropyl alchol, 69°-71° m.p.