BIS(2,2,2-TRIFLUOROETHYL) ETHER synthesis

13synthesis methods

Product Name:BIS(2,2,2-TRIFLUOROETHYL) ETHER
CAS Number:333-36-8
Molecular formula:C4H4F6O
Molecular Weight:182.06

75-89-8
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$9.00/1g

333-36-8
112 suppliers
$35.00/1 g

Yield:333-36-8 93.3%

Reaction Conditions:

Stage #1:2,2,2-trifluoroethanol with magnesium sulfate;sodium hydroxide at 60; for 5 h;
Stage #2: with thionyl chloride at -5 - 50; for 4 h;Inert atmosphere;Temperature;

Steps:

1-6 Example 1
In a 0.5 L reactor, 103 g (1 mol) of trifluoroethanol and 20 g (0.5 mol) were added.Sodium hydroxide, 0.1 g of water absorbing resin, 0.1 g of anhydrous magnesium sulfate,After the addition was completed, the temperature of the reaction vessel was controlled to be 60 ° C for 5 hours. The reaction system was taken out and suction filtered.The obtained filter cake was collected and placed in a vacuum drying oven at 150 ° C.2000Pa vacuum drying after 24h reuse;The filtrate was collected, placed in a reaction kettle containing a constant pressure dropping funnel, and protected with nitrogen for 1 hour.Then weighed 65g (0.55mol) of thionyl chloride and added it to the reaction kettle. The temperature was controlled at -5~5°C. After the addition was completed, the reaction was carried out at 5°C for 2h, and the temperature was raised to 50°C for 2h. The reaction was completed and the system was filtered. exceptThe sodium salt was dropped, and the filtrate was simply distilled to obtain 80 g of trifluoroethyl ether.The purity of the GC was monitored by 99.1%, and the yield was 93.3%.

References:

Shandong Yonghao New Materials Technology Co., Ltd.;Niu Huizhu CN109516900, 2019, A Location in patent:Paragraph 0017-0022

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