Carbon Disulfide → gallium tris(N,N-diethylcarbamodithioate)

HRID 354729

반응식

HRID 354729 반응식
[Cl-].[Ga+3:2].[Cl-].[Cl-].[CH2:5]([N:7]([CH2:11][CH3:12])[C:8](=[S:10])[S-:9])[CH3:6].[K+].[OH-].[K+].C(NCC)C.C(=S)=S>O1CCCC1>[CH2:5]([N:7]([CH2:11][CH3:12])[C:8](=[S:9])[S-:10])[CH3:6].[Ga+3:2].[CH2:5]([N:7]([CH2:11][CH3:12])[C:8](=[S:9])[S-:10])[CH3:6].[CH2:5]([N:7]([CH2:11][CH3:12])[C:8](=[S:9])[S-:10])[CH3:6]

참가 물질

7

반응물 5

HCID 6348Carbon DisulfideHCID 8021DiethylamineHCID 14797Potassium HydroxideHCID 186022Gallium monochloride2회HCID 23676196Potassium diethyldithiocarbamate

생성물 1

HCID 20480239gallium tris(N,N-diethylcarbamodithioate)

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7879abe971fd4e89b7e5b5654ec9da92
출처 데이터셋
uspto-grants-1983_03
특허 번호
US04377504

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