ChemicalBook CAS DataBase List METHYLDIFLUOROSILANE

METHYLDIFLUOROSILANE synthesis

13synthesis methods

Product Name:METHYLDIFLUOROSILANE
CAS Number:420-34-8
Molecular formula:CH4F2Si
Molecular Weight:82.12

2370-88-9 Synthesis

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Yield: 77%

Reaction Conditions:

with boron trifluoride diethyl etherate in toluene at 60 - 90; for 0.416667 h;

Steps:

4 Example 4: Synthesis of difluoromethylsilane, DFMS, by reaction of 2,4,6,8- tetramethylcyclotetrasiloxane with BF3
Example 4: Synthesis of difluoromethylsilane, DFMS, by reaction of 2,4,6,8- tetramethylcyclotetrasiloxane with BF3
(0088) An apparatus and procedure as described in Example 1 was used for Example 4. Thus, 2,4,6, 8-tetramethylcyclotetrasiloxane 16.07 g (66.8 mmol) and toluene 100.06 g (1.09 mol) were charged to the four neck flask. Boron trifluoride diethyl etherate (BF3- OEt₂) 26.24 g (184.9 mmol) was charged to the addition funnel. A dry ice/isopropanol slush bath was placed in the second addition funnel and in the bath under the two neck flask. BF3 - OEt₂ was added drop- wise to the reaction flask over 25 minutes. No reflux or significant exotherm was observed. The reaction mixture was then heated initially to 60°C, whereupon refluxing commenced, and subsequently further heated to 90°C. The volatile product was collected in the second (two neck) flask and subsequently transferred to a storage cylinder. The collected product fraction was determined to be DFMS by NMR analysis: 5¹⁹F = -138.50 ppm; δ = 4.85 ppm, ²J U-¹⁹F) = 69 Hz; δΗ^ = 0.47 ppm, ³J U-¹⁹F) = 6 Hz; = 3 Hz. The collected product (22.10 g) was 76 wt.% FDMS and thus the isolated yield was 77%

References:

ARKEMA INC.;SYVRET, Robert G.;POLSZ, Craig A. WO2016/32767, 2016, A1 Location in patent:Page/Page column 13

75-54-7 Synthesis