Method for producing carbonyl rest-containing organosilicon compounds
A technology of organosilicon compounds and compounds, applied in the direction of organic chemistry, chemical instruments and methods, compounds containing elements of group 3/13 of the periodic table, etc., can solve problems such as hindering large-scale production and loss
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Embodiment 1
[0937] 121 g of 3-hydroxypropyldimethylsilyl-terminated polydimethylsiloxane with an OH content of 3.2% were dissolved in 400 ml of dichloromethane, 1.90 g (11 mmol) of 4-hydroxy TEMPO, 50 Milliliters of saturated sodium bicarbonate solution and 2.27 grams (22 mmol) of sodium bromide were cooled to -10°C, under the strong stirring of anchor stirrer (2000rpm; RZR type stirrer of Heidolph Company), under the condition of thorough cooling 177 grams of industrial bleach (content about 1.8M, adjusted to pH 9.5 by adding 2N sulfuric acid) was added within 200 seconds. In this case, a suspension-like white mixture is formed in which small droplets of silicone oil with an average particle size of about 100 to 150 μm are dispersed in the continuous aqueous phase. After about 5 minutes, the phases separate and the organic phase containing the product is examined by NMR spectroscopy. Yield (standard analysis): 96% Si-bonded 2-formylethyl, 4% unreacted hydroxypropyl.
[0938] The compar...
Embodiment 2
[0941] 121 g of 3-hydroxypropyldimethylsilyl-terminated polydimethylsiloxane with an OH content of 1.25%, 950 mg (5.5 mmol) of 4-hydroxy-TEMPO, 50 ml of saturated bicarbonate Sodium solution and 1135 mg (11 mmol) of sodium bromide were cooled to -10°C, and 77 grams of industrial bleach solution (content was about 1.9M) was quickly added under conditions of vigorous stirring and thorough cooling, and the pH was adjusted by adding 2N sulfuric acid to 9.5). After about 15 minutes, the phases separate and the organic phase containing the product is examined by NMR spectroscopy. Yield (standard analysis): 95% Si-bonded 2-formylethyl, 5% unreacted hydroxypropyl.
Embodiment 3
[0943] The reaction of Example 2 was repeated with the difference that 100 g of polydimethylsiloxane with trimethylsilyl end groups functionalized with 3-hydroxypropyl groups in the side chain and further defined in Table 1 were used. Alkanes, where 4-hydroxy-TEMPO, saturated NaHCO 3 The amounts of solution, sodium bromide, and bleach used are listed in the table. At the end of the reaction, the reaction mixture was neutralized with 10% strength HCl(aq) (pH=6 to 7). After separation of the phases of the organosilicon compound, removal of all volatile constituents in vacuo and filtration, polydimethylsiloxane with trimethylsilyl end groups functionalized in the side chain with formylethyl groups is obtained. alkanes, which are essentially colorless clear oils.
[0944] Example
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