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.
Related Products of 4858-85-9, A common heterocyclic compound, 4858-85-9, name is 2,3-Dichloropyrazine, molecular formula is C4H2Cl2N2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
In a 100 mL three-necked flask, under N2 protection,Add magnesium chips (0.729g, 30mmol),Add 1 iodine (initiator),Add 10 mL of dry THF to immerse the magnesium chips,Start stirring,Add 2,3-dichloropyrazine (0.148 g, 1 mmol),Heating causes the reaction,THF reflux,The color of the iodine particles fades,Magnesium turnings indicate brightening,Lead to success.Stop heating,A solution of 2,3-dichloropyrazine in THF (4.291 g, 29 mmol, dissolved in 20 mL of dry THF) was slowly added dropwise.After the drop is over,Heated back to 65 degrees CelsiusFlow 1h.Get a new format reagent,The concentration is about 1 mol/L.At 100mLIn an eggplant-shaped bottle,JoinTetrabutylammonium chloride (0.278 g, 1 mmol),Under N2 protection,Slowly add the previously prepared format reagent (15mL, 15mmol).Stir at room temperature for 10 min,Then add diethylene glycol dimethyl ether (2.012g,15mmol),After stirring for 30 min at room temperature,Cool down to 0 to 5 degrees Celsius,A solution of 4-methylimino-N-2-pyridine-benzamide in THF (2.251 g, 10 mmol, 1.0 M in THF) was slowly added.After the addition was completed, the reaction solution was gradually warmed to room temperature for 2 h.After completion of the reaction, the reaction was quenched with 5 mL of aqueous hydrogen chloride (10%).Add 150 mL of a saturated aqueous solution of sodium bicarbonate,Extract twice with 100 mL of ethyl acetate.The organic layers were combined and washed with a saturated aqueous solution of sodium chloride.Dry over anhydrous sodium sulfate for 1 h,Dry under reduced pressure to obtain a crude product.Column chromatography with ethyl acetate/petroleum ether (1:2) gave 4-[amino-(3-chloro-2-pyridin2.82 g of pyrazinylmethyl]-N-(2-pyridyl)benzamide,The yield was 85% and the purity was 98%.
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; Anqing Qichuang Pharmaceutical Co., Ltd.; Wu Xueping; Chu Yijie; Chen Yao; Wang Min; (10 pag.)CN109020977; (2018); A;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem