Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 41663-84-7, name is 2-Methyl-5-nitroisoindoline-1,3-dione, A new synthetic method of this compound is introduced below., Computed Properties of C9H6N2O4
Example 12Conversion of Treated 4NPI to BisimideA 2-liter, 5-necked oil jacketed glass vessel, equipped with a Dean and Stark receiver topped with a reflux condenser, a mechanical stirrer, and means for maintaining a nitrogen atmosphere, was charged with 335 g (1.63 mol) of 4-NPI in 1000 g of toluene (resulting from the bicarbonate treatment of the 4NPI/water slurry, see above), and 6.2 g (0.008 mol HEG-Cl) of a catalyst solution composed of 34.4% by wt. HEG-Cl, 10.0% sodium chloride, and 55.6% water. An additional 500 g of toluene was added. The solution was brought to reflux using an external hot oil unit set at 120 C. to supply hot oil to the jacket of the vessel, and the water was removed by azeotropic distillation. Approximately 500 g of toluene was removed during the distillation. The dry 4-NPI/catalyst toluene solution was then added via a flexible fitting to a 5-liter, 5-necked oil jacketed glass vessel (equipped with a Dean and Stark Receiver topped with a reflux condenser, mechanical stirrer, and means for maintaining a nitrogen atmosphere) containing 222 g (8.15 mol) of BPA disodium salt and 700 g of toluene (the salt solution can also be added to the NPI solution). The temperature on the 5-liter vessel was maintained at 120 C. using a hot oil recirculating unit. HPLC of the reaction mixture indicated that the displacement reaction was complete in 60 min. to afford a 99.4% yield of BPA bisimide. The mixture was cooled to 80 C. and extractively purified with three 580 mL portions of 1% aqueous sodium hydroxide to afford pure bisimide with a yellowness index (YI) of 2.0.The YI was measured with a Macbeth 7000 spectrometer using ASTM D-1925. A blank of methylene chloride was measured for YI prior to measurement of the sample. This YIblank measurement was recorded for use in correcting the final measurement. About 0.5 g of a sample was dissolved into 10 mL of methylene chloride. The sample was then filtered through a 0.5 g HPLC filter. The mixture was then transferred to a 3.7 cm×5 cm×10 mm path length cell. The cell was placed into the calorimeter (ASTM D11925) and the YI was determined.The equation (I) below was used to correct the YI. This equation (I) is general and allows for solutions to also be measured for YI.YIcor=(YImeas-YIblank)*0.5*100/(wt. Sample in G*% solids of the sample) (I) The washes were done at 80 C., with a 5 minute agitation time and a 7 minute settling time. The YI of the material was 2.2. The YI of a typical reaction (without bicarbonate treatment of the 4NPI/water slurry) is 3 to 4.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; SABIC Innovative Plastics IP B.V.; US2009/292128; (2009); A1;,
Indoline – Wikipedia,
Indoline | C8H9N – PubChem