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ChemicalBook CAS DataBase List 1,4-BIS(3-AMINOPROPYLDIMETHYLSILYL)BENZENE
20152-18-5

1,4-BIS(3-AMINOPROPYLDIMETHYLSILYL)BENZENE synthesis

2synthesis methods
-

Yield:20152-18-5 92%

Reaction Conditions:

in methanol;5,5-dimethyl-1,3-cyclohexadiene;

Steps:

1 Example 1

Example 1 A 1-liter glass flask equipped with a stirrer, reflux condenser, thermometer and dropping funnel was charged with 201.5 g (1.0 mol) of N,N-bis(trimethylsilyl)-allylamine and 0.33 g of a 3% xylene solution of platinum 1,3-divinyltetramethyldisiloxane complex. To the flask kept at 60 to 65° C., 97.2 g (0.5 mol) of 1,4-bis-(dimethylsilyl)benzene was added dropwise over 3 hours from the dropping funnel. The reaction solution was allowed to ripen for 2 hours. 192.0 g (6.0 mol) of methanol was added to the reaction solution, which was kept under reflux for reaction for 6 hours. From the reaction solution, a fraction of 163 to 165° C. at 1 mmHg was collected in a yield of 142.0 g by vacuum distillation. By mass spectroscopy (MS), nuclear magnetic resonance spectroscopy (NMR), and infrared absorption spectroscopy (IR), the compound thus obtained was identified to be 1,4-bis(3-aminopropyldimethylsilyl)benzene (yield 92%). Also, by gas chromatography, the compound was found to be free of isomers. MS: m/z (attribution) 308 (molecular ion (M+) peak) 293 (M+-CH3 ion peak) 116 (Si(CH3)2(CH2CH2CH2NH2) ion peak)

References:

US6274754,2001,B1

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