The synthetic route of Ethyl 2,3-dicyanopropanoate has been constantly updated, and we look forward to future research findings.
Electric Literature of 40497-11-8, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 40497-11-8, name is Ethyl 2,3-dicyanopropanoate belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.
300L glass lined kettle add 80.142kg of absolute ethanol, stir,Then add 30.1% hydrogen chloride ethanol 45.579kg (containing hydrogen chloride 376.273mol), Configured to about 11% hydrogen chloride ethanol,Then add 98.0% 2,6-dichloro-4-trifluoromethylaniline 47.060kg (200.504mol),Control temperature 30 40 , after stirring and dissolving,Add 98.0% ethyl 2,3-dicyanopropionate 31.026kg (199.838mol), stir well,It is prepared as a raw material liquid and stored at about 20 .Add 25.136 kg of absolute ethanol to the axial-flow stirring tank, stir, and add 16.523 kg (234.704 mol) of 98.0% sodium nitrite, keeping the stirring configuration as a suspension.Pass the frozen brine at about 0 C into the reactor casing described in Example 1 above, and adjust the flow rate of the frozen brine after normal circulation. Then, the raw material liquid described in this example was pumped into the reactor described in Example 1 with a diaphragm metering pump at a flow rate of 5.00 l / min, and the suspension liquid in this example was pumped using a diaphragm metering pump at a flow rate of 1.00 l / min. Into the reactor described in Example 1, the reactor outlet was connected to a 500L glass-lined kettle. The flow rate of frozen brine is adjusted to control the temperature of the first stage of the reactor at 10-15 C, the temperature of the second stage at 15-20 C, and the temperature of the third stage at 20-25 C. Monitor the pH value and nitrite concentration, fine-tune the suspension flow, control the nitrite concentration at the outlet of the reactor to 0.1 to 0.5%, and the pH value to 1 to 5, after starting the discharge,Sampling HPLC to detect 2,6-dichloro-4-trifluoromethylaniline content of 0.169% (Figure 1, 12.329min is the raw material peak).After continuing to feed until the material is pumped, add 50 liters of 10% hydrogen chloride ethanol to the 300L mentioned in this example, add 10 liters of absolute ethanol to the stirring tank, and continue to use 5.00 liters / min and 1.00 liters / min. The partial flow rate is pumped into the reactor. After the pumping is completed, the contents of the reactor are purged with nitrogen.
The synthetic route of Ethyl 2,3-dicyanopropanoate has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Jiangsu Youpu Biochemical Technology Co., Ltd.; Zhang Jiqian; Shi Yunyun; Ma Chenglong; Jiang Fei; Gu Jialin; (10 pag.)CN111018786; (2020); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts