%0 Journal Article %T 溴水催化还原的α,α,α-三溴甲基酮类化合物的高选择性控制脱溴反应研究
Study on Highly Selective Control of Debromination Reaction of α,α,α-Tribromomethyl Ketones Catalyzed by Bromine Water %A 伊力努热·热夏提 %A 储向龙 %A 曾竟 %A 阿布都热西提·阿布力克木 %J Hans Journal of Chemical Engineering and Technology %P 241-251 %@ 2161-8852 %D 2022 %I Hans Publishing %R 10.12677/HJCET.2022.124032 %X 以1,4-二氧六环为溶剂,通过调节溴水溶液的质量和反应温度,实现了α,α,α-三溴甲基酮的高选择性还原脱溴。以中等至良好的收率合成了α,α-二溴甲基酮和α-一溴甲基酮。该反应具有广泛的底物和官能团耐受性,为α,α-二溴甲基酮和α-单溴甲基酮衍生物的合成提供了新途径。以α,α,α-三溴甲基酮(0.1 mmol)为反应底物,在80℃下1,4-二氧六环溶剂中加入20 mg溴水(Br2 (3.2 mg),H2O (16.8 mg))作为还原剂可得到产率为86%的α,α-二溴甲基酮。在α,α,α-三溴甲基酮类化合物的单次脱溴反应中,发现反应温度和溴水质量对α-一溴甲基酮的合成产生重大影响。因此,在本实验中,我们不断调整溴水的质量,调整反应温度,实现选择性合成α-一溴甲基酮。以α,α,α-三溴甲基酮(0.1 mmol)为原料,30 mg溴水(Br2 (4.8 mg),H2O (25.2 mg))为催化剂,温度120℃,在1,4-二氧六环溶剂中可得到收率77%的α-一溴甲基酮。
Using 1,4-dioxane or tetrahydrofuran as a solvent, the highly selective reductive debromination of α,α,α-tribromomethyl ketones was achieved by adjusting the quality of bromine water solution and reaction temperature. The α,α-dibromomethyl ketones, α-monobromomethyl ketones, and methyl ketones with moderate to good yields were synthesized. This reaction has a wide range of substrates and functional group tolerance, providing a new pathway for the synthesis of α,α-dibromomethyl ketone, α-monobromomethyl ketone methyl ketone derivatives. With α,α,α-Tribromomethyl ketone (0.1 mmol) was used as the reaction substrate, and 20 mg of bromine water (Br2 (3.2 mg), H2O (16.8 mg)) was added to 1,4-dioxane solvent at 80?C as the reducing agent to obtain a product with a yield of 86% α,α-Dibromomethyl ketone. In the single debromination reaction of tribromomethyl ketone compounds, it was found that the reaction temperature and the quality of bromine water were important to the synthesis of α-bromomethyl ketone and have a significant impact. The synthesis of Dibromomethyl ketones can have a significant impact. Therefore, in this experiment, we constantly adjust the quality of bromine water, adjust the reaction temperature, and realize selective synthesis α-Bromomethyl ketone. With α,α,α-tribromophenone (0.1 mmol) as the raw material, 30 mg of bromine aqueous solution, Br2 (4.8 mg) as a catalyst, H2O (25.2 mg)), the temperature being 120?C, a 77% yield can be obtained within a 1,4-dioxane solvent α-Monobromomethyl ketone. %K 溴水,α¸ %K α¸ %K α-三溴甲基酮,选择性脱溴
Bromine Water %K α¸ %K α¸ %K α-Tribromomethyl Ketones %K Selective Debromination %U http://www.hanspub.org/journal/PaperInformation.aspx?PaperID=53391