Reference of 2112-22-3,Some common heterocyclic compound, 2112-22-3, name is 2,3-Dichloro-6-nitrobenzonitrile, molecular formula is C7H2Cl2N2O2, 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.
2,3-dichloro-6-nitrobenzonitrile, 500 gm, was dissolved in 7500 ml of THF in a clean dry RB flask maintaining a nitrogen blanket. 139.3 am of sodium borohydride was added at 25-30 C. The suspension was cooled to 15-20 C. 653 gms of Borontrifluoride etherate was added to the reaction mixture over a period of about 2 hours while maintaining the temperature between 15-30 C. After the addition was complete, the temperature was raised about 65 C. and maintained at reflux for 2 hours. The reaction mixture was cooled to about 0-5 C. A mixture of 2.0 liter water and 200 ml concentrated HCl was slowly added to the reaction mixture while maintaining the temperature below 20 C. After the addition was complete, THF was distilled from the reaction mixture under vacuum maintaining temperature below 50 C. The reaction mixture was cooled to about 10-15 C. and 2.0 liter ethylacetate was added. The pH of reaction mixture was adjusted to 10-11 using 25% aqueous sodium hydroxide solution while maintaining the temperature below 15 C. The ethylacetate layer was separated and concentrated to about half the original volume. The reaction mixture was cooled to 15-20 C. and 500 ml IPA-HC1 was added slowly, maintaining temperature below 30 C. After cooling to about 0-5 C., the solids obtained were filtered and washed with 500 ml chilled ethylacetate. The solids were dried to obtain 2,3-dichloro-6-nitrobenzyl amine hydrochloride (450 gms),
The synthetic route of 2112-22-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; WATSON PHARMA PRIVATE LIMITED; US2010/305318; (2010); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts