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ChemicalBook CAS DataBase List N-Methyl-N,N-bis(2-pyridylethyl)amine
5452-87-9

N-Methyl-N,N-bis(2-pyridylethyl)amine synthesis

5synthesis methods
-

Yield: 65%

Reaction Conditions:

with ammonium chloride in toluene at 85 - 86; for 60 h;

Steps:

Samples
Betahistine dihydrochloride was obtained from LEBSA(Espinos Y Bofill S. A. laboratories). Impurities 3 and 4were acquired from Sigma-Aldrich. Impurity C1 (6) wasobtained by preparative chromatography purification.Mobile phases constituted of (A) aqueous formic acid(0.1%) solution and (B) methanol (0.1% formic acid).Pumps programming: 5 to 13.3% of A in 10 min. Peaks withretention time (tR) of 7.8 min was collected. Compound 5was synthesized by following a known procedure:31compound 1 (0.05 g, 3.7 mmol), toluene (2.5 mL), and4-vinylpiridine (3) were placed inside a 10-mL roundbottomflask. Ammonium chloride (10 mg, 0.19 mmol)was added, and the mixture was stirred in an oil bath at85-86 °C for 60 h. The mixture was then purified by flashchromatography; methylene chloride/methanol (6:1) wasused as eluent. Yield: 65% of colorless oil.

References:

de Mello, Murilo B.M.;De Oliveira, Antonio A.F.;De Oliveira, Caroline L.;Ultramari, Mariah A.;Gama, Fernando H.S.;Mascarello, Alessandra;Guimarães, Cristiano R.W.;de Freitas, Miller N.;Cunha, Carlos E.;Lourenço, Tiago C.;Ferreira, Fernanda P.;Lopes, João L.C.;Clososki, Giuliano C. [Journal of the Brazilian Chemical Society,2019,vol. 30,# 7,p. 1415 - 1424]

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