Diselenide and its preparation method, selenium-containing surfactant and its preparation method, application
A technology of surfactant and diselenide, applied in chemical instruments and methods, non-central analgesics, skin care preparations, etc., can solve the problems of poor stability and color, and achieve good light transmittance and chromaticity , high product conversion rate, and low acute toxicity of aquatic organisms
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Embodiment 1
[0043] 1) Synthesis of diselenide starter: slowly drop the DMF solution of 17.9kg 4-bromocyclohexanol (4-bromocyclohexanol 4-bromocyclohexanol content 10wt%) under argon protection Add to the aqueous solution of 40.8kg sodium diselenide (sodium diselenide content 5wt%), add Cu 2 O(50-250nm) and TiO 2 The mass ratio of (50-150nm) is 3:1 composite catalyst, the amount of catalyst added is 11.49g, and vigorously stirred at room temperature for 6h. The reaction solution was extracted with ether in multiple stages, and the solvent was evaporated under reduced pressure to obtain a crude product, which was recrystallized from ethanol to obtain the target compound. 13 C NMR (500MHz, DMSO-d6): δ=69.2 (s, 2C, CH-OH), 39.3 (s, 2C, CH-Se), 33.6 (s, 4C; CH2), 32.4 (s, 4C; CH2 ). HRMS-ESI: m / z: 357.9948 (calcd. for [M+H]+, 357.9950).
[0044]2) Synthesis of selenium-containing surfactant: add 300 g of the diselenide initiator synthesized above and 1.65 g of KOH solid catalyst into the r...
Embodiment 2
[0046] 1) Synthesis of diselenide initiator: slowly dropwise the DMF solution (4-bromocyclohexanol content 15wt%) of 12.53kg 4-bromocyclohexanol to 21.42kg diselenide In the aqueous solution of sodium (sodium diselenide content is 10wt%), add Cu 2 O(250-500nm) and TiO 2 The mass ratio of (150-500nm) is 4:1 composite catalyst, the addition amount of catalyst is 32.172g, stir vigorously at room temperature for 8h. The reaction solution was extracted with ether in multiple stages, and the solvent was evaporated under reduced pressure to obtain a crude product, which was recrystallized from ethanol to obtain the target compound. 13 C NMR (500MHz, DMSO-d6): δ=69.4(s, 2C, CH-OH), 38.3(s, 2C, CH-Se), 33.8(s, 4C; CH2), 32.3(s, 4C; CH2 ). HRMS-ESI: m / z: 357.9952 (calcd. for [M+H]+, 357.9950).
[0047] 2) Synthesis of selenium-containing surfactants: add 300g initiator and 6g sodium methoxide / methanol solution (sodium methoxide content 30w.t.%) to the reaction vessel and heat up to ...
Embodiment 3
[0049] 1) Synthesis of diselenide initiator: slowly dropwise the DMF solution (4-bromocyclohexanol content 20wt%) of 10.74kg 4-bromocyclohexanol to 13.6kg diselenide In the aqueous solution of sodium (sodium diselenide content is 15wt%), add Cu 2 O(50-250nm) and TiO 2 The mass ratio of (150-500nm) is 5:1 composite catalyst, the addition amount of catalyst is 4.2g, stir vigorously at room temperature 10h. The reaction solution was extracted with ether in multiple stages, and the solvent was evaporated under reduced pressure to obtain a crude product, which was recrystallized from ethanol to obtain the target compound. 13 C NMR (500MHz, DMSO-d6): δ=68.4(s, 2C, CH-OH), 38.5(s, 2C, CH-Se), 33.4(s, 4C; CH2), 32.6(s, 4C; CH2 ). HRMS-ESI: m / z: 357.9951 (calcd. for [M+H]+, 357.9950).
[0050] 2) Synthesis of selenium-containing surfactants: add 300 g of initiator and 0.72 g of phosphazene catalyst to the reaction vessel, heat up to 105° C., vacuum dehydration; control the reaction...
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