三苯基硅醇

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Triphenylsilanol (22 g) and 80 g (0.45 mol) of 3,5,5-trimethyl-4-hydroxy-4-ethynylcyclohex-2-en-1-one and 1.6 g of stearic acid are dissolved in 800 ml of xylene, treated with 1.92 ml of vanadium isopropylate and heated to reflux temperature while stirring. After 31/2 hours the reaction mixture is cooled and washed with 5% sodium bicarbonate, whereby an emulsion results. The organic phase is then separated, the emulsion is also separated and extracted with ether. The organic phases are dried over magnesium sulphate and concentrated. The residue (117.9 g) is distilled (oil bath 130°-170°; 0.001 mm Hg). In this manner there are obtained 51.8 g (64.8%) of (2,6,6-trimethyl-4-oxo-2-cyclohexen-1-ylidene)acetaldehyde (Z:E=about 3:1). heated to reflux temperature After 31/2 hours the reaction mixture is cooled washed with 5% sodium bicarbonate, whereby an emulsion results The organic phase is then separated the emulsion is also separated extracted with ether The organic phases are dried over magnesium sulphate concentrated The residue (117.9 g) is distilled (oil bath 130°-170°; 0.001 mm Hg)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Bistriphenylsilyl chromate is usually used as the catalyst of unsaturated hydrocarbon compound polymerization such as ethylene polymerization. With respect to its synthesis process, early in 1958, U.S. Pat. 7,863,891 disclosed a process wherein bistriphenylsilyl chromate can be obtained with a yield of 85% by reacting triphenylsilanol and chromium trioxide in glacial acetic acid at 50° C. for 10 minutes. L. M. Bakert et al disclosed a process wherein bistriphenylsilyl chromate can be obtained with a yield of about 60% by reacting triphenylsilanol and chromium trioxide in carbon tetrachloride at room temperature for 24 hours [J. Org. Chem., Vol. 85, No. 8, pp. 774-776, March 1970]. The former Czechoslovakia Patent CS 175856 disclosed a process wherein bistriphenylsilyl chromate can be obtained with a yield of 43-71% by reacting triphenylsilanol or triphenylsilyl ether and chromium trioxide in acetonitrile or propyl cyanide. However, the starting material triphenylsilanol used in the above processes is obtained by the hydrolysis of triphenylchlorosilane, so the process for the preparation of bistriphenylsilyl chromate is relatively complicated and the yield thereof is relatively low. The former Soviet Union Patent SU 689192 .disclosed a process wherein bistriphenylsilyl chromate can be obtained with a yield of 94% by reacting triphenylchlorosilane and potassium dichromate in glacial acetic acid at 40°-50° C. for 1.5 hours. The reaction equation thereof is as follows: ##STR1## With respect to its synthesis process can be obtained with a yield of 85% at 50° C. for 10 minutes can be obtained with a yield of about 60% at room temperature for 24 hours can be obtained with a yield of 43-71%

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Triphenylsilanol (22 g) and 80 g (0.45 mol) of 3,5,5-trimethyl-4-hydroxy-4-ethynylcyclohex-2-en-1-one and 1.6 g of stearic acid are dissolved in 800 ml of xylene, treated with 1.92 ml of vanadium isopropylate and heated to reflux temperature while stirring. After 31/2 hours the reaction mixture is cooled and washed with 5% sodium bicarbonate, whereby an emulsion results. The organic phase is then separated, the emulsion is also separated and extracted with ether. The organic phases are dried over magnesium sulphate and concentrated. The residue (117.9 g) is distilled (oil bath 130°-170°; 0.001 mm Hg). In this manner there are obtained 51.8 g (64.8%) of (2,6,6-trimethyl-4-oxo-2-cyclohexen-1-ylidene)acetaldehyde (Z:E=about 3:1). heated to reflux temperature After 31/2 hours the reaction mixture is cooled washed with 5% sodium bicarbonate, whereby an emulsion results The organic phase is then separated the emulsion is also separated extracted with ether The organic phases are dried over magnesium sulphate concentrated The residue (117.9 g) is distilled (oil bath 130°-170°; 0.001 mm Hg)