Synthetic Route of 1824-81-3, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 1824-81-3 as follows.
An alkali trap, an equal pressure dropping funnel, a thermometer, and a mechanical stirrer were attached to a 1000 mL four-necked round bottom flask. (A) 2-amino-6-picoline (27.0 g 0.25 mol) and 48% HBr (125 mL 2.31 mol) were placed in this reaction vessel. The reaction vessel was immersed in an ice bath and cooled to 0 C. Br2 (37.5 mL 0.72 mol) was transferred to an equal pressure dropping funnel, The temperature of the reaction solution was kept at 0 C. and slowly dropped into the reaction vessel over 90 minutes while vigorously stirring with a mechanical stirrer. NaNO 2 (42.5 g 0.62 mol) was weighed and dissolved in about 100 mL of distilled water. This was transferred to an equal pressure dropping funnel,While stirring vigorously with a stirrer, it dripped over about 2 hours. At this time, care was taken that the temperature of the reaction solution did not exceed 10 C. In order to complete the reaction, NaNO 2 (2.50 g 0.036 mol) was dissolved in about 10 mL of distilled water and added, It was confirmed that nitrogen gas was not generated from the reaction vessel. While cooling in an ice bath, NaOH (95.0 g, 2.4 mol) was dissolved in about 300 mL of distilled water, after cooling sufficiently, it was gradually added to the solution for neutralization. At this time, care was taken that the temperature of the reaction solution did not exceed 20 C. The reaction mixture was extracted with Et 2 O (200 mL × 4) and the organic layer was collected. Anhydrous Na 2 SO 4 was added and dried, Upon concentration, a brown oily substance was obtained. This oily substance was distilled under reduced pressure in a rectifying tube, fractionated at 55 C. to 60 C. at a reduced pressure degree of 7.00 mmHg, A yellow oily substance was obtained. This material was stored at -40 C. Yield: 72% (32.0 g)
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,1824-81-3, its application will become more common.
Reference:
Patent; THE DOSHISHA; KODERA, MASAHITO; TSUJI, TOMOKAZU; (18 pag.)JP2017/197451; (2017); A;,
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