[Bis (trihydrocarbyl silyl) amino silyl] functionalized styrene and preparation method thereof
A technology of styrene derivatives and alkyl groups, which is applied in chemical instruments and methods, organic chemistry, compounds of group 4/14 elements of the periodic table, etc., can solve problems such as hydrolytic instability of aniline derivatives
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Embodiment 1
[0078] Magnesium metal (13.37 g, 0.55 mol) was loaded into a 1 L volumetric reactor equipped with a magnetic stirrer, dropping funnel and reflux condenser with gas introduction accessory and oil valve (Zaitsev gasket) under an argon atmosphere, followed by addition of Dry and deoxygenated tetrahydrofuran (THF, 200 mL) and iodine (I 2 , 0.69g, 2.75mmol). Next, it was heated to 50° C. with stirring the contents of the reactor. Magnesium activation was performed until the brown color disappeared, then the reactor contents were allowed to cool to room temperature. Then, 1-[{N,N-bis(trimethylsilylamino)}(dimethylsilyl)]-2-{chloro-dimethylsilyl}ethane (170.10 g, 0.50 mol) and the remainder of the solvent (300 mL) were added to the prepared activated magnesium. The dropping funnel was filled with 1-bromo-4-vinylbenzene (99 g, 0.53 mol). In the initial step of the reaction, 9.90 mL of 1-bromo-4-vinylbenzene was added dropwise to the mixture without stirring the reactor contents. ...
Embodiment 2
[0085] A 20 L volume reactor equipped with a magnetic stirrer, dropping funnel and reflux condenser with gas introduction accessories and oil valve (Zaitsev gasket) was loaded with magnesium metal (153.73 g, 6.2232 mol) in an argon atmosphere, followed by addition of Dry and deoxygenated tetrahydrofuran (THF, 1.00L) and iodine (I 2 , 7.97g, 31.62mmol). Next, it was heated to 50° C. with stirring the contents of the reactor. Magnesium activation was performed until the brown color disappeared, then the reactor contents were allowed to cool to room temperature. Then, 1-[{N,N-bis(trimethylsilylamino)}(dimethylsilyl)]-2-{chlorodimethylsilyl}ethane (1956.20 g, 5.75 mol) was mixed with The remaining portion (9.00 L) of solvent was added to the prepared activated magnesium. The dropping funnel was filled with 1-bromo-4-vinylbenzene (1,105 g, 6.04 mol). In the initial step of the reaction, 100 mL of 1-bromo-4-ethylbenzene was added dropwise into the reaction system without stirrin...
Embodiment 3
[0087] In the same manner as in Example 1, in 6.19g (0.26mol) with I 2(0.38 g, 1.16 mmol) in the presence of activated Mg to make 1-[{N,N-bis(trimethylsilylamino)}(dimethylsilyl)]-2-{chlorodimethylsilyl } Ethane (78.82 g, 0.23 mol) was reacted with 1-(chloromethyl)-4-vinylbenzene (37.13 g, 0.24 mol). 91.03 g of 1-[{N,N-bis(trimethylsilylamino)}(dimethylsilyl)]-2-{(4-vinylphenylmethyl)dimethylsilyl} were obtained Ethane, the yield is 93%. The product was subjected to spectroscopic analysis.
[0088] GC-MS:
[0089] 393.2(0.9); 260.2(3.4); 237.4(2.0); 236.4(10.3); 234.5(41.4); 223.5(2.6); 222.5(12.7); 221.6(19.1); 188.8(1.4);186.8(1.5);177.8(1.7);176.9(2.3);175.9(14.8);1517(7.5);117.7(3.9);100.5(2.6);73.3(2.8).
[0090] NMR:
[0091] 1 H NMR (300MHz, CDCl 3 , 300K) δ (ppm) = 7.28 (d, 2H, -C 6 h 4 -); 6.97(d, 2H, -C 6 h 4 -); 6.67 (dd, 1H, -CH=); 5.68 (d, 1H, =CH 2 ); 5.68 (d, 1H, =CH 2 ); 5.16 (d, 1H, =CH 2 ); 2.11(s, 2H, -CH 2 -); 0.51, 0.43 (m, 4H, -CH 2 CH 2 ...
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