PROPARGYLTRIMETHYLSILANE synthesis
- Product Name:PROPARGYLTRIMETHYLSILANE
- CAS Number:13361-64-3
- Molecular formula:C6H12Si
- Molecular Weight:112.25
Yield:13361-64-3 66%
Reaction Conditions:
Stage #1:propargyl bromide with magnesium;mercury dichloride in diethyl ether;toluene at -20 - 0;Inert atmosphere;Reflux;
Stage #2:chloro-trimethyl-silane in diethyl ether;toluene at 0 - 20; for 4.5 h;
Steps:
* Compound (A) preparation exampleSynthesis of compound 3 - 30
magnesium chips (7.2g), HgCl2(90 mg), 80% propargyl toluene solution (1 ml) and 50 ml anhydrous ethyl ether (Na processing new distillation) under the protection of nitrogen by adding 1000 ml three-neck bottle and stirring, exothermic reaction begins to be slowly heated to reflux, then adding 100 ml ethyl ether system is cooled to -20 °C, maintain -20 °C dropwise 80% propargyl toluene solution (32 ml) and 150 ml of a mixed solution of ethyl ether, after dropping the temperature to 0 °C reaction 2h. Maintain 0 °C, dropwise trimethylchlorosilane (38 ml) and 110 ml ethyl ether of the mixed solution, after dropping in 0 °C reaction 0.5h temperature to room temperature reaction 4h. System producing a large amount of magnesium salt, filtering, the filtrate is first rectification column for separating a large amount of ether solvent, re-distillation collection 90 - 92 °C-poly isobutylene. GC - MS detection for alkyne propyl trimethyl silane and toluene mixture, propargyl trimethyl silane 3 - 30 content 80%, yield of about 66%.
References:
Henan Agricultural University;Liu Jia;Na Risong;Li Honglian;Wang Changqing;Liu Bingshan;Feng Xianli;You Xiufeng;Sun Shujun;Lu Shichao CN106674228, 2017, A Location in patent:Paragraph 0084; 0085; 0086
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