5325-94-0, Ethyl piperidine-1-carboxylate is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
In nitrogen atmosphere, to a 500 ml three-neck flask, 16.7 g (77.6 mmol) of 4-bromo-2,6-dimethylanisole, and 150 ml of dehydrated diethyl ether were added. While the mixture was cooled in a methanol/dry ice bath, 49.7 ml (81.5 mmol) of a n-butyllithium/hexane solution (1.64 M) was gradually added. While the temperature was gradually elevated to room temperature, the mixture was stirred for 16 hours. While the mixture was cooled in an ice bath, a solution composed of 4.83 g (30.7 mmol) of N-carboethoxypiperidine and 50 ml of dehydrated diethyl ether was gradually added with a dropping funnel over a period of 20 minutes. The mixture was stirred for 1 hour at room temperature, and stirred for 2 hours under heating to reflux. Thereto, in an ice bath, 100 ml of 2N hydrochloric acid was gradually added. The resultant two-layer solution was transferred to a 500 ml separating funnel. The resultant solution was shaken several times. Thereafter, the aqueous layer was removed. Subsequently, the organic layer was washed two times with 100 ml of water, one time with 100 ml of a saturated aqueous sodium bicarbonate solution, and one time with 100 ml of a saturated saline solution, and dried over anhydrous magnesium sulfate for 30 minutes. After the solvent was distilled off under reduced pressure, a small amount of hexane was added to perform recrystallization to give a solid. This solid was washed with a small amount of hexane, and dried under reduced pressure. As a result, 6.83 g (22.9 mmol, 74.5%) of 4,4′-dimethoxy-3,3′,5,5′-tetramethylbenzophenone was obtained as a white solid. 4,4′-Dimethoxy-3,3′,5,5′-tetramethylbenzophenone was identified by 1H NMR spectrum. Measured values thereof are shown below. 1H NMR spectrum (270 MHz, CDCl3): delta/ppm 7.44 (s, 4H), 3.77 (s, 6H), 2.31 (s, 12H), 5325-94-0
5325-94-0 Ethyl piperidine-1-carboxylate 21399, apiperidines compound, is more and more widely used in various fields.
Reference£º
Patent; MITSUI CHEMICALS, INC.; Endo, Koji; Hiwara, Mayumi; Matsuura, Sadahiko; Kosugi, Yoko; Yamamura, Yuichi; Mizobuchi, Yusuke; (50 pag.)US9969827; (2018); B2;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem