Dichloroacetic acid methyl ester synthesis
- Product Name:Dichloroacetic acid methyl ester
- CAS Number:116-54-1
- Molecular formula:C3H4Cl2O2
- Molecular Weight:142.97
79-36-7
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116-54-1
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Yield:116-54-1 94.3%
Reaction Conditions:
in hydrogenchloride
Steps:
4 Preparation of methyl dichloroacetate (MDA)
30 dm3 of DAC were present in excess in the reactor throughout the entire reaction, there was a vigorous production of HCl gas right from the start. In the present case, the stirred kettle was provided with a column and attached glass condensers through which the HCl gas was released. Any entrained product was retained in the condensers and dripped back into the reaction vessel. For safety reasons, the unit was operated in such a way that the pressure of HCl gas in the unit did not exceed 1.2 bar. After about 7.5 hours, the total amount of DAC of 2590 dm3 (including the 30 dm3 initially introduced) DAC [sic] had reacted with 1100 dm3 of methanol. This point was signalled by a cessation of HCl production and a drop in the pressure in the unit. To complete the reaction, a further 50 dm3 of methanol were then metered in and the whole mixture was stirred for 15 minutes. The reaction mixture was subsequently distilled under vacuum to give 3650 kg of MDA, this being a yield of 94.3% based on DAC.
References:
Hoechst Aktiengesellschaft US5292928, 1994, A
67-56-1
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1768-31-6
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67-66-3
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116-54-1
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$5.00/5 g