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 platinumdivinylmethyldisiloxane (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 nun Hg. 1H NMR 300 MHz, CDCl3 :δ6 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 =7HZ,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=7HZ), 5.75* (AXY,JAX=18 Hz, JAY=7 Hz), 1.09* (d, 0.1 H), 1.07(d,l.5 H), 0.67 (m 1.2 H), 0.47 (m 1.2 (H), 0.12, (m, 0.1 H), 0.08, (s, 1H), 0.06, (s, 1 H) , 0.05 (s, 5 H) . 13C NMR 75 MHz, CDCl3 : δ135.089,, (CH); 134,628, (CH); 134,4, (CH2); 10.137, (CH 2); 6.869,, (CH); 4.21,, (CH2); 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 NaC1): 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