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 40117-63-3,Quinuclidine-4-carboxylic acid hydrochloride, as follows.40117-63-3
To a stirred suspension of quinuclidine-4-carboxylic acid hydrochloride (5.5 g) in 30 mL of dry THF at 0 C. was added borane dimethyl sulfide complex (6.7 g, 3 eq.). The reaction mixture was stirred at room temperature for 1 hr and heated to reflux for 16 hr. It was then quenched with drop-wise addition of methanol (7 mL) at 0 C. The solvent was then removed under reduced pressure, and the crude product obtained was purified by column chromatography (Silica gel, 20% EA:Hexane) to afford the product quinuclidin-4-ylmethanol N-borane complex as a white solid (1.35 g, 30%).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, Quinuclidine-4-carboxylic acid hydrochloride, and friends who are interested can also refer to it.
Reference£º
Patent; CoMentis, Inc.; BILCER, Geoffrey M.; NG, Raymond; (104 pag.)US2016/9706; (2016); A1;,
Quinuclidine – Wikipedia
Quinuclidine | C7H13N | ChemSpider