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ChemicalBook CAS DataBase List 2,2-Difluoroethanol
359-13-7

2,2-Difluoroethanol synthesis

14synthesis methods
2,2-Difluoroethyl Acetate

1550-44-3

2,2-Difluoroethanol

359-13-7

Example 13: Synthesis of 2,2-difluoroethanol from ethyl 2,2-difluoroacetate (Step b2) In a 0.5 L glass reactor equipped with a mechanical stirrer, reflux condenser and temperature probe, 164 g of ethyl 2,2-difluoroacetate (GC purity 95%), 106 g of methanol, and 3 g of solid NaOH were added. the reaction was carried out at 65 °C for 2 h until the conversion was complete. The 2,2-difluoroethanol was isolated by distillation to give 96.3% GC purity and 87% isolated yield.

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Yield:359-13-7 93.3%

Reaction Conditions:

with hydrogen at 110; under 3750.38 - 15001.5 Torr; for 4 h;Autoclave;Temperature;Pressure;

Steps:

5
CuO-ZnO-BaO / CNT catalyst 2 prepared in Example 2 was usedA difluoroethanol was prepared by hydrogenation of difluoroacetate,In a stainless steel autoclave, 35 g of ethyl difluoroacetate and 2 g of catalyst 2 were placed,Closed reactor, the use of 0.5MPa hydrogen replacement kettle air, the introduction of hydrogen pressure of 2MPa,Heating up to 110 ° C with stirring,Reaction 4 h. Cooling down, until the temperature dropped to 25 after the pressure, open the reactor,After the reaction solution was taken out, the catalyst was separated from the reaction solution, the filtrate was distilled at atmospheric pressure and the pellets were collected at 97 to 99 ° C,21.5 g of difluoroethanol was obtained, the yield was 93.3%, and the purity was 99%.

References:

Shandong Dongyue PolymerMaterial Co., Ltd.;CHEN, YUE;LUO, YONGZHEN;BI, ZUOWEI CN105461512, 2016, A Location in patent:Paragraph 0042-0043

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