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ChemicalBook CAS DataBase List 4-Bromo-N,N-dimethylaniline
586-77-6

4-Bromo-N,N-dimethylaniline synthesis

13synthesis methods
-

Yield:586-77-6 85%

Reaction Conditions:

with 0.72 KNaX-BS zeolite at 150; for 1 h;Reagent/catalyst;

Steps:

Methylation of anilines with dimethyl carbonate. General procedure.
General procedure: Into a pressure microreactor of stainless steel of 17 mL capacity or into a glass ampule (20 mL) (results of the parallel runs were virtually identic) was charged 5-10 wt % of catalyst (0.94HY-BS, NaY-BS, 0.72KNaX-BS), 100 mmol of aniline or its derivative, and 400 mmol of dimethyl carbonate. The reactor was hermetically closed (the ampule was sealed), and was heated for 1-4 h at 150 °C. After the end of the run the reactor was cooled to room temperature, opened, the reaction mixture was filtered through a bed of Al2O3. Dimethyl carbonate was distilled off, the residue was distilled at atmospheric pressure or in a vacuum, or crystallized from ethanol.

References:

Khusnutdinov;Shchadneva;Mayakova, Yu. Yu.;Ardieva;Khazipova;Kutepov [Russian Journal of Organic Chemistry,2016,vol. 52,# 11,p. 1565 - 1570][Zh. Org. Khim.,2016,vol. 52,# 11,p. 1574 - 1578,5]

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