Reaktion #954573

ord-c0c2774e1bd34ab18cd78baa8dbd464c

Reaktionsgleichung

Cl[Si](Cl)(c1ccccc1)c1ccccc1
dichlorodiphenylsilane
CC(C)(C)c1cc(Sc2cc(C(C)(C)C)cc(C(C)(C)C)c2O)c(O)c(C(C)(C)C)c1
2,2'-thiobis(4,6-di-tert-butylphenol)
CCN(CC)CC
triethylamine
CC(C)(C)c1cc2c(c(C(C)(C)C)c1)O[Si](c1ccccc1)(c1ccccc1)Oc1c(cc(C(C)(C)C)cc1C(C)(C)C)S2
white solid
Ausbeute 43.3%
CC(C)(C)c1cc2c(c(C(C)(C)C)c1)O[Si](c1ccccc1)(c1ccccc1)Oc1c(cc(C(C)(C)C)cc1C(C)(C)C)S2
2,4,8,10-Tetra-tert-butyl-6,6-diphenyl-dibenzo[d,g][1,3,6,2]dioxathiasilocin
Ausbeute 43.3%

Lösungsmittel

Reaktionsbedingungen

Temperatur
92°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeas evidenced by the disappearance of the phenolic absorption in the IR spectrum
  2. 2
    SonstigeThe triethylamine hydrochloride is removed by filtration
  3. 3
    Sonstigethe solvent is removed in vacuo
  4. 4
    SonstigeThe residue is recrystallized from 2-butanone

Vorschrift

A solution of 12.66 grams of dichlorodiphenylsilane in 50 ml of toluene at 5°-10° C. is added dropwise to a solution of 22.14 grams of 2,2'-thiobis(4,6-di-tert-butylphenol) and 10.12 grams of triethylamine in 100 ml of toluene. The reaction mixture is heated at 92° C. until the reaction is complete as evidenced by the disappearance of the phenolic absorption in the IR spectrum. The triethylamine hydrochloride is removed by filtration and the solvent is removed in vacuo. The residue is recrystallized from 2-butanone to give 13.49 grams (43%) of a white solid: mp 202°-205° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04775497uspto-grants-1988_10