1-(chloromethoxy)octane

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

実験手順: The precursor, C8H17OCH2OC4H8OH was prepared by monoalkylation of butane diol with octyl chloromethyl ether. The precursor was first acetylated with acetyl chloride in methylene chloride containing triethylamine and then fluorinated, and a portion of the crude perfluorinated product was hydrolyzed by treatment with aqueous sulfuric acid and then distilled to yield the carboxylic acid C8F17OCF2OC3F6CO2H, having a boiling range 100°-106° C. at 1.1 torr. Differential scanning calorimetry revealed the acid had a Tg of -97.0° C. and several crystalline exotherms of -77.4, -61.5 and -37.7° C. and a broad melting point at -9.0° C. distilled

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

実験手順: The precursor, C8H17OCH2OC4H8OH was prepared by monoalkylation of butane diol with octyl chloromethyl ether. The precursor was first acetylated with acetyl chloride in methylene chloride containing triethylamine and then fluorinated, and a portion of the crude perfluorinated product was hydrolyzed by treatment with aqueous sulfuric acid and then distilled to yield the carboxylic acid C8F17OCF2OC3F6CO2H, having a boiling range 100°-106° C. at 1.1 torr. Differential scanning calorimetry revealed the acid had a Tg of -97.0° C. and several crystalline exotherms of -77.4, -61.5 and -37.7° C. and a broad melting point at -9.0° C. distilled

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

実験手順: The precursor, C8H17OCH2OC4H8OH was prepared by monoalkylation of butane diol with octyl chloromethyl ether. The precursor was first acetylated with acetyl chloride in methylene chloride containing triethylamine and then fluorinated, and a portion of the crude perfluorinated product was hydrolyzed by treatment with aqueous sulfuric acid and then distilled to yield the carboxylic acid C8F17OCF2OC3F6CO2H, having a boiling range 100°-106° C. at 1.1 torr. Differential scanning calorimetry revealed the acid had a Tg of -97.0° C. and several crystalline exotherms of -77.4, -61.5 and -37.7° C. and a broad melting point at -9.0° C. distilled

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

実験手順: The precursor, C8H17OCH2OC4H8OH was prepared by monoalkylation of butane diol with octyl chloromethyl ether. The precursor was first acetylated with acetyl chloride in methylene chloride containing triethylamine and then fluorinated, and a portion of the crude perfluorinated product was hydrolyzed by treatment with aqueous sulfuric acid and then distilled to yield the carboxylic acid C8F17OCF2OC3F6CO2H, having a boiling range 100°-106° C. at 1.1 torr. Differential scanning calorimetry revealed the acid had a Tg of -97.0° C. and several crystalline exotherms of -77.4°, -61.5° and -37.7° C. and a broad melting point at -9.0° C. distilled

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

実験手順: The precursor, C8H17OCH2OC4H8OH was prepared by monoalkylation of butane diol with octyl chloromethyl ether. The precursor was first acetylated with acetyl chloride in methylene chloride containing triethylamine and then fluorinated, and a portion of the crude perfluorinated product was hydrolyzed by treatment with aqueous sulfuric acid and then distilled to yield the carboxylic acid C8F17OCF2OC3F6CO2H, having a boiling range 100°-106° C. at 1.1 torr. Differential scanning calorimetry revealed the acid had a Tg of -97.0° C. and several crystalline exotherms of -77.4°, -61.5° and -37.7° C. and a broad melting point at -9.0° C. distilled

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

実験手順: The precursor, C8H17OCH2OC4H8OH was prepared by monoalkylation of butane diol with octyl chloromethyl ether. The precursor was first acetylated with acetyl chloride in methylene chloride containing triethylamine and then fluorinated, and a portion of the crude perfluorinated product was hydrolyzed by treatment with aqueous sulfuric acid and then distilled to yield the carboxylic acid C8F17OCF2OC3F6CO2H, having a boiling range 100°-106° C. at 1.1 torr. Differential scanning calorimetry revealed the acid had a Tg of -97.0° C. and several crystalline exotherms of -77.4°, -61.5° and -37.7° C. and a broad melting point at -9.0° C. distilled

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

実験手順: 33 g (1.1 mole) of (CH2O)n were stirred in 100 ml 1,1,2-trichloroethane with 130 g (1.0 mole) 1-octanol at 0°-5° C. HCl gas was passed for one hour. The product was analysed by MS-GC, as described in example 7 and was found to contain 2.3% bis-chloromethylether.

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

実験手順: 75 g (2.5 mole) of paraformaldehyde were stirred in 250 ml 1,1,2-trichloroethane with 268 ml (2.5 mole) 1-octanol at 0°-5° C. HCl gas was passed for one hour. The product chloromethyloctyl ether can be isolated by evaporation of the excess solvent. Alternatively, a stock solution of 3M concentration is made in 1,1,2-trichloroethane and used as such, or kept refrigerated. Chloromethyloctylether may be distilled, b.p. 63°-64° C. (0.7 torr).