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ChemicalBook CAS DataBase List Benzonitrile, 5-amino-2-methoxy- (9CI)
214623-57-1

Benzonitrile, 5-amino-2-methoxy- (9CI) synthesis

3synthesis methods
-

Yield: 82%

Reaction Conditions:

with palladium 10% on activated carbon;hydrogen in methanol at 20; for 0.5 h;

Steps:

5 5-amino-2-methoxybenzyl cyanide
The 2-methoxy-5-nitrobenzyl cyanide (1eq, 220mg, 1.23mmo1), 20mL of methanol, 10mg of palladium on carbon (10% of mass) were added sequentially in to the 100mL round bottom flask, the bottle connected to the three links, reaction was stirred at room temperature. Vacuum pumping then recharging N2 , repeat this cycle for 3 times , and N2 loading time not less than 5 min. the reaction was allow to react for 30min at room temperature under H2 protection. After the reaction was complete in 30mins , the palladium-carbon was filtered, concentrated, and column chromatography separation (PE: EA = 5: 1) to give 150 mg of product as a white crystalline solid (compound 7). Yield 82%.

References:

Chinese Academy Of Sciences Shanghai Pharmaceutical Institute;Long Yaqiu;Xu Zhongliang;Wang Heyao;Cai Mengxin CN106892871, 2017, A Location in patent:Paragraph 0109; 0112; 0113