Reaktion #1952957

ord-3a3c2972154e416caa086e85612cc210

Reaktionsgleichung

CN(CC(O)CN(C)S(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F)S(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F
[C4F9SO2N(CH3)CH2]2CHOH
CCO[Si](CCCN=C=O)(OCC)OCC
OCN(CH2)3Si(OCH2CH3)3
CCO[Si](CCCNC(=O)OC(CN(C)S(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F)CN(C)S(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F)(OCC)OCC
[C4F9SO2N(CH3)CH2]2CHOC(O)NH(CH2)3Si(OCH2CH3)3

Lösungsmittel

Reaktionsbedingungen

Temperatur
30°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeA three-necked round bottom 500 mL flask fitted with a stirrer
  2. 2
    Temperaturheating mantle, condenser, nitrogen inlet, Dean-Stark trap and thermometer
  3. 3
    TemperaturThe mixture was heated
  4. 4
    Sonstigeapproximately 50 g of material was removed
  5. 5
    TemperaturThe mixture was heated at 75° C. under nitrogen for 16 hours

Vorschrift

A three-necked round bottom 500 mL flask fitted with a stirrer, heating mantle, condenser, nitrogen inlet, Dean-Stark trap and thermometer was charged with [C4F9SO2N(CH3)CH2]2CHOH (204.6 g, 0.300 mol), and methyl ethyl ketone (250 g). The mixture was heated and approximately 50 g of material was removed using the Dean-Stark trap. The mixture was cooled to 30° C., and OCN(CH2)3Si(OCH2CH3)3 (74.4 g, 0.301 mol) and three drops of stannous octanoate were added. The mixture was heated at 75° C. under nitrogen for 16 hours. A clear, slightly yellow product ensued. Analysis of the product was consistent with [C4F9SO2N(CH3)CH2]2CHOC(O)NH(CH2)3 Si(OCH2CH3)3.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07629298B2uspto-grants-2009_12