Some common heterocyclic compound, 383-62-0, name is Ethyl 2-chloro-2,2-difluoroacetate, molecular formula is C4H5ClF2O2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. category: esters-buliding-blocks
TEOF (130 g, 0.88 mol) was placed in a flask equipped with a magnetic stirring bar and a vacuum distillation cooler. ECDFAA (35 g, 0.175 mol) was added. The resulting mixture was heated to 110C (outer temperature of the flask) under a mild vacuum (300 mbar) ; ethanol formed during the reaction is slowly distilled out of the vessel. After 2h, the starting material was completely consumed, and product formation was observed by GC analysis. Excess of TEOF was removed from the reaction mixture by distillation (at 100C, starting with a pressure of 100 mbar at the beginning and 10 mbar at the end, to remove all TEOF traces), resulting pure product as pale yellow liquid with quantitative yield. 1H NMR (500 MHz, CHLOROFORM-d) delta ppm 1.15 (t, 3 H) 1.20 (t, 3 H) 1.27 (t, 3 H) 3.49 – 3.57 (m, 1H) 3.61 – 3.69 (m, 1H) 3.71 – 3.79 (m, 2 H) 4.23 (q, 2 H) 4.34 (d, J=8.24 Hz, 1 H) 5.18 (d, J=8.24 Hz, 1 H).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 383-62-0, its application will become more common.
Reference:
Patent; SOLVAY SA; Januzems, Janis; EP2644598; (2013); A1;,
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