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ChemicalBook CAS DataBase List Morpholine, 4,4'-carbonylbis
38952-62-4

Morpholine, 4,4'-carbonylbis synthesis

13synthesis methods
-

Yield:38952-62-4 93%

Reaction Conditions:

in dichloromethane at 0 - 20;Inert atmosphere;

Steps:

General procedure A for the synthesis of urea (2b-d)

General procedure: To a solution of amine (5-10 equiv) in anhydrous dichloromethane (25 mL) at 0 °C was added dropwise a solution of triphosgene (1 equiv) in anhydrous dichloromethane (5 mL). The reacting mixture was stirred at 0 °C for 1 h and then stirred at room temperature for additional 4 h. After completion, water (100 mL) was added to dissolve the precipitate. The aqueous layer was extracted with dichloromethane (2 × 25 mL). The combined organic layers were washed with 1 N HCl (25 mL), saturated NaHCO3 (25 mL) and brine (25 mL). The solution was dried (Na2SO4) and concentrated to give the desired product of satisfying purity (>95%) for use in the next step.

References:

Donnier-Maréchal, Marion;Goyard, David;Folliard, Vincent;Docsa, Tibor;Gergely, Pal;Praly, Jean-Pierre;Vidal, Sébastien [Beilstein Journal of Organic Chemistry,2015,vol. 11,p. 499 - 503] Location in patent:supporting information