Reaction #355382

ord-81ea3c2daeef44fc84dad99817c11ee7

Reaction equation

N#C[S-].[K+]
potassium thiocyanate
CCCCO[Si](CCCCl)(OCCCC)OCCCC
3-chloropropyl tri-n-butoxy silane
[Cl-].[K+]
potassium chloride
CCCCO[Si](CCCSC#N)(OCCCC)OCCCC
3-thiocyanatopropyl tri-n-butoxy silane
Yield 85.0%

Solvents

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Otherwas separated off with a Seitz
  2. 2
    Filtrationfilter
  3. 3
    workup.DISTILLATIONThe solvent was distilled off from the filtrate
  4. 4
    workup.DISTILLATIONthe 3-thiocyanatopropyl tri-n-butoxy silane distilled in vacuo
  5. 5
    Other0.1 128°-129° C., yield 85%

Procedure

24.3 grams of potassium thiocyanate were dissolved in 900 ml. of n-butanol and the solution heated to boiling. Then there were added dropwise in about 30 minutes 81.3 grams of 3-chloropropyl tri-n-butoxy silane. After a further 20 hours of boiling at reflux temperature the precipitated potassium chloride was separated off with a Seitz filter. The solvent was distilled off from the filtrate and the 3-thiocyanatopropyl tri-n-butoxy silane distilled in vacuo. B.P. 0.1 128°-129° C., yield 85% based on the weight of the 3-chloropropyl tri-n-butoxy silane.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US03947436uspto-grants-1976_03