3-ACRYLAMIDOPROPYLTRIS(TRIMETHYLSILOXY)SILANE, tech-95 synthesis

Yield:115258-10-1 92%

Reaction Conditions:

with sodium carbonate in water;

Steps:

1

In a 100 mL three-necked flask equipped with a thermometer, a dropping funnel and a nitrogen inflow instrument, and a magnetic stirring bar therein, were put 1 mole of [(CH₃)₃SiO]₃Si(CH₂)₃NH₂, 1.05 moles of acrylic acid chloride and 2.0 moles of sodium carbonate in an aqueous 10% solution and stirred. Subsequently, the mixture was washed with water, filtrated through a paper filter and, then, volatile materials were distilled off under a reduced pressure to obtain a colorless product which was solid at room temperature and had a melting point of 51 degrees C. A molecular structure of the product obtained was analyzed by ¹H-NMR and IR to find that the product was a silicone compound represented by the following formula. The yield was 92%. The ¹H-NMR spectra and IR spectra are as described below. [0080] ¹H-NMR (400 MHz, CDCl₃): δ 0.09 (s, 27H), 0.45-0.50 (m, 2H), 1.59 (quin., J=7.0 Hz, 2H), 3.32 (q, J=7.0 Hz, 2H), 5.58 (brs, 1H), 5.62 (dd, J=10.3, 1.4 Hz, 1H), 6.06 (ddd, 17.0, 8.4, 1.4 Hz, 1H), 6.25 (dd, 17.0, 10.3 Hz, 1H) [0081] IR(ATR): ν 753, 835, 1041, 1248, 1408, 1556, 1625, 1655, 2958, 3285.

References:

US2015/87853,2015,A1 Location in patent:Paragraph 0078-0081