反应 #969870

ord-10f2fcad1aa541e785d7dd1d597df23d

反应方程式

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

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他A three-necked round bottom 500 ml flask fitted with a stirrer
  2. 2
    温度heating mantle, condenser, nitrogen inlet, Dean-Stark trap and thermometer
  3. 3
    其他about 50 grams of material was removed
  4. 4
    温度The mixture was cooled to about 30° C.
  5. 5
    温度The resulting mixture was heated at about 75° C. under nitrogen for about 16 hours

实验过程

Next, [C4F9SO2N(CH3)CH2]2CHOC(O)NH(CH2)3Si(OCH2CH3)3 was prepared as follows. 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 about 204.6 grams of the [C4F9SO2N(CH3)CH2]2CHOH (0.3 mol), and about 250 grams methyl ethyl ketone. The mixture was heated for about 1 hour at about 100° C. and about 50 grams of material was removed using the Dean-Stark trap. The mixture was cooled to about 30° C., and about 74.4 grams of OCN(CH2)3Si(OCH2CH3)3 (0.3 mol), and three drops of stannous octanoate were added. The resulting mixture was heated at about 75° C. under nitrogen for about 16 hours.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08236737B2uspto-grants-2012_08