In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 5-Amino-4H-1,2,4-triazole-3-carboxylic acid, other downstream synthetic routes, hurry up and to see.
Adding a certain compound to certain chemical reactions, such as: 3641-13-2, name is 5-Amino-4H-1,2,4-triazole-3-carboxylic acid, belongs to triazoles compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 3641-13-2, category: Triazoles
Example 1 – Preparation of an Azo Compound; In this example the desired pH for the coupling reaction between a diazotised amine and a coupling component was a pH in the range 7 to 9.(a) Preparation of Coupling Component StreamNaphthalene-2-hydroxy-3,6-disulphonylamino-4-benzoic acid (0.91 mol) was dispersed in water (8.3kg). Once charging was complete, the pH was adjusted to 7-8 using 47% sodium hydroxide solution. Agitation was continued until dissolution was complete. The volume was made up to 9.2L by the addition of further water as required.(b) Preparation of Amine and Nitrite Solution3-Amino-1,2,4-triazole-5-carboxylic acid (1.27mol) was dissolved in water (2.9kg) at 45C, pH 9. The pH was maintained at 9 to 10 by addition of 47% sodium hydroxide solution as required. The solution was cooled to room temperature and sodium nitrite (1.33mol) was added. Stirring was continued until dissolution was complete. The volume was made up to 3.2L by the addition of further water as required.(c) Continuous Manufacture of Desired ProductThe reaction apparatus consisted of a number of feed vessels and pumps, two reactors, a product hold tank (or “buffer vessel”) and containers for the collection of product.The first reactor was a small continuous stirred tank reactor for the production of the diazonium salt. This reactor was assembled such that the overflow (i.e. outlet) stream from this reactor would flow into the second reactor.The second reactor consisted of a length of flexible tubing arranged in a “loop”. Into this loop were fitted a centrifugal recirculation pump, a flow meter, a pH sensor, inlet ports for diazonium salt, coupling component stream and sodium hydroxide stream for pH adjustment and an exit port for the desired chemical compound. A flow meter and inlet port for diazonium salt were positioned downstream of the recirculation pump and the exit port was positioned still further downstream, such that the majority of the tubing length lay between the inlet port for the diazonium salt and the exit port. The exit port was located at the highest point of the loop reactor. The coupling component and sodium hydroxide inlet ports, and a pH sensor, were fitted between the exit port and the inlet (“suction side”) of the recirculation pump.Prior to start-up, the loop reactor was filled with water and the recirculation pump was started. The flow rate was adjusted to approximately 4 litres per minute (approximately 240L/h) at the outlet of the recirculation pump. The exit port was initially directed to a waste receiver. The reagent feed pumps were set to the correct flow rates as given below and the diazonium salt precursors, coupling component and sodium hydroxide solution were charged to the appropriate feed vessels.A small amount of sodium hydroxide was then fed into the loop to raise the pH to pH to approximately pH 10. The coupling component feed pump was started, such that coupling component stream entered the loop. The flow was allowed to continue until coupling component was present throughout the loop and the pH had stabilised at 8.5-9.5. The coupling component pump was then stopped.The agitator in the first reactor (where the diazonium salt will be prepared) was switched on. The amine / sodium nitrite feed and hydrochloric acid feed pumps were started, giving flows of 7.7 litres per hour and 4.2 litres per hour respectively of the amine/nitrite solution and the hydrochloric acid solution into the first reactor to form a diazonium salt. The first reactor was allowed to fill.Once the first reactor had filled, the coupling component feed pump was restarted (giving a flow of 22.1 litres per hour) and diazonium salt slurry formed in the first reactor was allowed to flow into the loop reactor. Via the inlet port. The pH of the coupling component in the loop reactor was maintained at approximately 9 by feeding in sodium hydroxide at an appropriate rate (a variable speed pump and pH controller were used to achieve this). A distinct colour change was observed to spread through the loop reactor from the diazonium salt inlet port, indicating the formation of the desired chemical compound (an azo dye). The desired chemical compound overflowed from the loop reactor via the exit port at a rate of approximately 37 litres per hour. The recycled flow therefore exceeded the throughput by a factor of approximately 6, therefore the Recirculation Ratio was about 6. This recycled stream of desired chemical compound provided pH buffering for subsequent cycles of the loop, such that the desired chemical compound was obtained consistently at approximately pH8.It was found that the loop reactor took a few residence times to achieve steady state, so the first 2.5 litres of product were discarded and the second 2.5 litres were collected and analysed separately from the bulk.The desired chemical compound was obtained in good yield and purity.
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 5-Amino-4H-1,2,4-triazole-3-carboxylic acid, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; AVECIA INKJET LIMITED; WO2006/8495; (2006); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics