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ChemicalBook CAS DataBase List 1-Chloro-1-methylsilacyclopentane

1-Chloro-1-methylsilacyclopentane synthesis

4synthesis methods
-

Yield:2406-31-7 55%

Reaction Conditions:

with magnesium;ethylene dibromide in dibutyl diglyme at 20 - 95; for 5 h;Grignard Reaction;

Steps:

7

Example 7: Preparation of l-Chloro-l-methyl-l-silacyclopentane23Og of magnesium (Mg) powder and 15Og of dibutyl diglyme were placed in a 12-liter three-necked round-bottom flask. The flask was equipped with a dropping funnel, a thermometer and a water condenser fitted with a gas inlet supplied with dry nitrogen. 508g of 1,4- dichlorobutane and 598g of methyltrichlorosilane were mixed with 3000g of dibutyl diglyme in the dropping funnel. Several drops of 1 ,2-dibromoethane were added to the flask to initiate the Grignard reaction. Once the reaction was initiated, the silane/dichlorobutane/dibutyldiglyme mixture was charged through the dropping funnel and the reaction was stirred mechanically. The reaction was cooled by an external cold-water bath. The mixed raw materials were added at a speed to maintain the reaction at a temperature in the range of approximately 500C to approximately 950C. All of the mixed raw materials were added within 3 hours. The reaction was further stirred at room temperature for 2 hours after the addition of raw materials. The resultant mixture from the reaction separated into two phases after standing at room temperature. The top organic phase was isolated. Distillation of the organic phase under reduced pressure yielded approximately 55% to approximately 70%of 1-chloro-l -methyl- 1-silacyclopentane.

References:

WO2008/33980,2008,A2 Location in patent:Page/Page column 11