反应详情

温度

70 °C

To the 25 ml round bottomed flask equipped with a reflex condenser was charged 10.17 g of tetravinylsilane (75 mmol), 1 g of 1,1,3,3-tetramethyldisiloxane (7.5 mmol) and 10 μL of platinum-divinylmethyldisiloxane (5% Pt). The mixture was stirred and heated at 70° C. until it turned light yellow. (Scheme 5). From this mixture, 0.88 g (29% yield) of 1,3-di-[2-(trivinylsilyl)ethyl]-1,1,3,3-tetramethyldisiloxane (7) was isolated by distillation at 115° C. and 0.1 mm Hg. 1H NMR 300 MHz, CDCl3 :δ 6.22** (AXY,JAX =18 Hz, JAY =2 Hz Z.Z H), 6.20** (AXY, JAX =18 Hz, JAY =2 Hz), 6.15 (AXY,JAX =18Hz, JAY =2 Hz), 6.12 (AXY,JAX =7 Hz, JAY =2 Hz), 6.11* (AXY, JAX =7 Hz, JAY =2 Hz), 6,08** (AXY,JAX =7 Hz, JAY =2 Hz), 6.07** (AXY,JAX =7 Hz, JAY =Hz), 5.82** (AXY,JAX =18 Hz, JAY =7 Hz), 5.80* (AXY,JAX =18 Hz, JAY =7 Hz), 5.79 (AXY,JAX =18 Hz, JAY =7 Hz), 5.76** (AXY,JAX =18 Hz, JAY =7 Hz), 5.75* (AXY,JAX =18 Hz, JAY =7 Hz), 1.09** (d, 0.1 H), 1.07* (d,1.5H), 0.67 (m 1.2H), 0.47 (m 1.2 (H), 0.12* (m, 0.1H), 0.08* (s, 1H), 0.06* (s, 1H), 0.05 (s, 5H). 13NMR 75 MHz, CDCl3 :δ 135.089*, (CH); 134,628, (CH); 134,4, (CH2); 10.137, (CH2); 6.869*, (CH); 4.21*, (CH 2); 4.131, (CH2); 1.347*, (CH3); -0.34, (CH3). 29Si NMR 99.4 MHz, CDCl3 with Cr(acac)3 δ-18.12, 8.00. IR (neat liquid on NaCl): cm-1 3180(w), 3050(s), 3010(m), 2960(s), 2910(m), 2880(m), 2790(w), 1610(m), 1400(s), 1250(s), 1130(s), 1050(s), 1010(s), 955(s), 840(s), 800(m), 770(s), 730(s), 625(W), 550(m), 525(m). C20H/38Si4O calc. C 59.04, H 9.41, Si 27.61, 0 3.96; found C 57.76, H 9.02. ##STR11##

1. customTo the 25 ml round bottomed flask equipped with a reflex condenser