Ethyl difluoroacetate synthesis
- Product Name:Ethyl difluoroacetate
- CAS Number:454-31-9
- Molecular formula:C4H6F2O2
- Molecular Weight:124.09
Yield:454-31-9 96%
Reaction Conditions:
with N,N-dimethyl acetamide for 4 h;Product distribution / selectivity;Inert atmosphere;Sealed tube;Cooling with ice;
Steps:
2
The same operation as in Example 1 was performed except for using 55 g (1.2 mol) of ethanol, 208 g (2.4 mol) of DMAc and 129 g (1.25 mol) of the difluoroacetic acid fluoride. There was thus obtained 392 g of a crude ethyl difluroacetate mixture (containing 208 g of DMAc) as a reaction liquid. The reaction liquid was distillated under reduced pressure (9.0 kPa) by a distillation column (theoretical plate number: 5 plates) packed with Dixon packing, thereby extracting 144 g of ethyl difluoroacetate (isolated yield: 96%) with a purity of 98.8 area% and a fluorine ion concentration of 0.07 mass% as a main fraction (column top temperature: 41.0°C) as shown in TABLE 1.
References:
EP2522652,2012,A1 Location in patent:Page/Page column 9
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