Synthesis method of DPA
A synthesis method and autoclave technology, applied in the field of DPA synthesis, can solve the problems of complex operation, long reaction time, low yield, etc., and achieve the effect of mild reaction conditions, short reaction time and simple operation
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[0010] (1) In a 200ml autoclave, add 4.7ml of o-nitrotoluene, 76.6ml of methanol, 2.7ml of distilled water, 0.02g of 3% Pt / C, seal the autoclave, replace the air with nitrogen for 3 times, and inject 0.1 Mpa of hydrogen, control the temperature at 50°C for 8 hours, stop the reaction, cool down to room temperature, take out the reaction solution and filter, distill off most of the methanol from the filtrate under reduced pressure, dilute the residual solution with water, neutralize the pH value with ammonia water to neutral , the upper organic phase was separated, the aqueous phase was extracted 3 times with ether, the organic phases were combined, and the organic phase was distilled under reduced pressure to remove fractions, the MMA purity was 98.9%;
[0011] (2) In a 200ml autoclave, add MMA26ml, phenol 106ml, cyclohexanone 4.2ml, 3% Pt / C0.28g, seal the autoclave, replace the air in the autoclave with nitrogen, and then adjust the nitrogen pressure to 1Mpa, control The tempe...
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