DICHLORO-METHYL-OCTADECYLSILANE

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

実験手順: The procedure is more specifically as follows. Octadecylmethyldichlorosilane [CAS No. 5157-75-5] (1500 g, i.e. 4.08 mol) in solution in anhydrous diethyl ether (250 mL) is added dropwise (90 min) to a mixture of water (345 g), triethylamine (1138 g) and diethyl ether (29 L) kept at a temperature between −2° C. and 6° C. The mixture is then stirred for 2 h at a temperature between 0° C. and 5° C. The precipitate formed is filtered, washed successively with 6 L of demineralized water, then 3 times with 4 L of demineralized water. The solid obtained is dried in the open air until it reaches a constant mass. Octadecylmethyldihydroxysilane or octadecylmethylsilanediol (1226 g) is thus obtained in the form of a white solid having a melting point of 87° C. with a yield of 91%, NMR analysis furthermore confirming the structure of the product obtained with a molar purity of 95%. kept at a temperature between −2° C. and 6° C The precipitate formed is filtered washed successively with 6 L of demineralized water The solid obtained is dried in the open air until it

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a 1 l four-neck flask with stirrer, reflux condenser and dropping funnel, 31.7 g of salicyl alcohol (0.25 mol) and 66.7 g (0.52 mol) of dried N-ethyldiisopropylamine were suspended under argon in 100 ml of anhydrous toluene at 22° C. 110 g of Octadecylmethyldichlorosilane (95%; 0.25 mol) was melted and dissolved in 100 ml of dry toluene. This solution was added dropwise at 23 to 27° C. within 55 minutes, in the course of which an exothermic reaction was observed. Cooling with an ice bath held the reaction temperature at a maximum of 27° C. After the addition had ended, the temperature was raised to 40° C., and exothermicity (without heating to 45° C.) was again observed. The reaction vessel was then cooled to 40° C. with cold water, and it was stirred at this temperature for one hour and then cooled to RT. The suspension was left to stand at RT overnight. The precipitate (hydrochloride) was filtered off with suction through a P40 glass frit under N2, and the filtrate was concentrated by rotary evaporation at 120° C./5 mbar. Yield 80.9 g (77% of theory). In a 1 l four-neck flask with stirrer, reflux condenser This solution was added dropwise at 23 to 27° C. within 55 minutes, in the course of which an exothermic reaction Cooling with an ice bath at a maximum of 27° C After the addition exothermicity (without heating to 45° C.) cooled to RT The suspension was left to stand at RT overnight The precipitate (hydrochloride) was filtered off with suction through a P40 glass frit under N2 the filtrate was concentrated by rotary evaporation at 120° C./5 mbar

反応条件: temp:45.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a 1 l four-neck flask with stirrer, reflux condenser and dropping funnel, 31.7 g of salicyl alcohol (0.25 mol) and 66.7 g (0.52 mol) of dried N-ethyldiisopropylamine were suspended under argon in 100 ml of anhydrous toluene at 22° C. Octadecylmethyldichlorosilane (95%) was melted and dissolved in 100 ml of dry toluene. This solution was added dropwise at 23 to 27° C. over 55 minutes, in the course of which an exothermic reaction was observed. By cooling with an ice bath, the reaction temperature was kept at not more than 27° C. After the addition had ended, the temperature was raised to 40° C., in the course of which exothermicity (without heating to 45° C.) was again observed. The reaction vessel was then cooled to 40° C. with cold water, and the mixture was stirred at this temperature for one hour and then cooled to RT. The suspension was left to stand at RT overnight. The precipitate (hydrochloride) was filtered off with suction under N2 through a P40 glass frit, and the filtrate was concentrated by rotary evaporation at 120° C./5 mbar. Yield 80.9 g (77% of theory) In a 1 l four-neck flask with stirrer, reflux condenser This solution was added dropwise at 23 to 27° C. over 55 minutes, in the course of which an exothermic reaction By cooling with an ice bath was kept at not more than 27° C After the addition cooled to RT The suspension was left to stand at RT overnight The precipitate (hydrochloride) was filtered off with suction under N2 through a P40 glass frit the filtrate was concentrated by rotary evaporation at 120° C./5 mbar

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

実験手順: The procedure is more specifically as follows. Octadecylmethyldichlorosilane [CAS No. 5157-75-5] (1500 g, i.e. 4.08 mol) in solution in anhydrous diethyl ether (250 mL) is added dropwise (90 min) to a mixture of water (345 g), triethylamine (1138 g) and diethyl ether (29 L) kept at a temperature between −2° C. and 6° C. The mixture is then stirred for 2 h at a temperature between 0° C. and 5° C. The precipitate formed is filtered, washed successively with 6 L of demineralized water, then 3 times with 4 L of demineralized water. The solid obtained is dried in the open air until it reaches a constant mass. Octadecylmethyldihydroxysilane or octadecylmethylsilanediol (1226 g) is thus obtained in the form of a white solid having a melting point of 87° C. with a yield of 91%, NMR analysis furthermore confirming the structure of the product obtained with a molar purity of 95%. kept at a temperature between −2° C. and 6° C The precipitate formed is filtered washed successively with 6 L of demineralized water The solid obtained is dried in the open air until it