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ChemicalBook CAS DataBase List Dimethylmorpholine
141-91-3

Dimethylmorpholine synthesis

8synthesis methods
-

Yield:141-91-3 95%

Reaction Conditions:

with ammonia;hydrogen at 200; under 150015 Torr;Reagent/catalyst;Temperature;

Steps:


General procedure: The amination of diols was carried out in standard flow setups consisting of a 200-cm3 stainless steel reactor equipped with an electrical heating jacket and a thermocouple pocket. The reactor was charged with 100-200 cm3 of the catalyst (grain size 1.5-3.0 mm) which was reduced with a hydrogen-nitrogen gas mixture over a period of 12 to 24 h at a temperature of up to 400°C. When the reduction was complete, the reactor was adjusted to a required temperature and a hydrogen pressure of 20.0 MPa, and hydrogen and ammonia were supplied at a flow rate of 25-50 and 60-400 L/h, respectively; the corresponding diol or its aqueous solution was then fed at a flow rate of 13-40 mL/h.

References:

Timofeev;Bazanov;Zubritskaya [Russian Journal of Organic Chemistry,2016,vol. 52,# 12,p. 1756 - 1761][Zh. Org. Khim.,2016,vol. 52,# 12,p. 1765 - 1770,6]

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