2-Trifluoromethyl-morpholine hydrochloride synthesis

Yield: 87%

Reaction Conditions:

with hydrogenchloride;palladium 10% on activated carbon;hydrogen in methanol;water for 3 h;Inert atmosphere;

Steps:

4.1.4 2-Trifluoromethylmorpholine hydrochloride (1*HCl)
General procedure: To a solution of amine 9 (62.7g, 256.0mmol) in methanol (400mL) concd HCl (50mL) and Pd/C (10%, 20.0g) were added. The mixture was vented off several times with Ar and stirred for 3h under atmosphere of H₂. The mixture was filtered off and evaporated to dryness. The residue was treated with a mixture of ether/ acetone (1:1, 200mL) and filtered off to yield pure 1 (43.1g, 225.0mmol, 87% yield) as a white solid, mp 187-188°C.

References:

Shcherbatiuk, Andriy V.;Shyshlyk, Oleg S.;Yarmoliuk, Dmytro V.;Shishkin, Oleg V.;Shishkina, Svitlana V.;Starova, Viktoriia S.;Zaporozhets, Olga A.;Zozulya, Sergey;Moriev, Roman;Kravchuk, Olga;Manoilenko, Olga;Tolmachev, Andrey A.;Mykhailiuk, Pavel K. [Tetrahedron,2013,vol. 69,# 19,p. 3796 - 3804]