反应 #3693065
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04377504
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: This compound was prepared by a double decomposition reaction between gallium chloride and potassium diethyldithiocarbamate. The former was purchased from a chemical supply house; the latter was synthesized as follows: to 43.0 g (0.769 moles) of potassium hydroxide and 56.3 g (0.769 moles) of diethylamine in a flask, 59.9 g (0.786 moles) of carbon disulfide was dropped dropwise while the flask was cooled in ice water. A solid product was formed from the combination of these reactants. It was dissolved in about 100 mL of tetrahydrofuran (THF), heated to the boiling point of THF, then cooled in ice water and solvent was removed by filtration. The nearly white crystalline product was washed with diethyl ether. When dry the resulting potassium diethyldithiocarbamate weighed 137.4 g. A solution containing 25.1 g (0.134 moles) of it in about 100 mL of THF was added to a cooled solution that contained 7.84 g (0.0445 moles) of gallium chloride in about 200 mL of THF. This mixture was refluxed for five hours, cooled, filtered, and the solid recrystallized from THF and n-hexane. Its composition, calculated as [(C2H5)2NCS2 ]3Ga, is 35.01 percent C, 5.89 percent H, 8.17 percent N, and 13.55 percent Ga; chemical analyses showed 35.79 percent C, 5.91 percent H, 8.29 percent N, and 6.9 percent Ga. The reason for the low concentration of gallium is not known. However, the concentration determined by the actual analysis provided the basis for calculating the quantity that was added to treat a cracking catalyst. the latter was synthesized A solid product was formed from the combination of these reactants solvent was removed by filtration The nearly white crystalline product was washed with diethyl ether When dry the resulting potassium diethyldithiocarbamate A solution containing 25.1 g (0.134 moles) of it in about 100 mL of THF was added to a cooled solution This mixture was refluxed for five hours cooled filtered the solid recrystallized from THF and n-hexane The reason for the low concentration of gallium However, the concentration provided the basis was added to treat a cracking catalyst
来源 ID: ord-7879abe971fd4e89b7e5b5654ec9da92