HRID354729

反应详情

EQUATION

反应方程式

HRID 354729 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. customthe latter was synthesized
  2. customA solid product was formed from the combination of these reactants
  3. customsolvent was removed by filtration
  4. washThe nearly white crystalline product was washed with diethyl ether
  5. dry with materialWhen dry the resulting potassium diethyldithiocarbamate
  6. additionA solution containing 25.1 g (0.134 moles) of it in about 100 mL of THF
  7. additionwas added to a cooled solution
  8. temperatureThis mixture was refluxed for five hours
  9. temperaturecooled
  10. filtrationfiltered
  11. customthe solid recrystallized from THF and n-hexane
  12. concentrationThe reason for the low concentration of gallium
  13. concentrationHowever, the concentration
  14. customprovided the basis
  15. additionwas added
  16. additionto treat a cracking catalyst