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ChemicalBook CAS DataBase List 3-Chloro-N,N-diMethylbenzaMide, 97%

3-Chloro-N,N-diMethylbenzaMide, 97% synthesis

6synthesis methods
-

Yield:24167-52-0 95%

Reaction Conditions:

with di-tert-butyl peroxide;copper(I) bromide in ethyl acetate at 120;

Steps:

Typical procedure for the preparation of N-substituted benzamides in the presence of CuBr and DTBP (TP)

General procedure: Benzoic acid (1.0 mml), tetramethylthiuram disulfide (TMTD) (1.1 mmol), CuBr (10% mmol), DTBP (di-tert-butyl peroxide, 2.0 equiv) were added in dried seal tube equipped with a septum and magnetic stirrer bar, EtOAc (ethyl acetate, 2 mL) was then added. The mixture was stirred at 120 oC and checked by TLC until the starting material was finished (about 10-12 h). The reaction was cooled down to room temperature, quenched with sat. NH4Cl solution (5 mL) and then extracted with ethyl acetate (10 mml). The crude solution was dried over anhydrous Na2SO4 and evaporated under vacuum. The residue was purified by flash column chromatography to afford the desired product.

References:

Zeng, Meng-Tian;Xu, Wan;Liu, Min;Liu, Xing;Chang, Cai-Zhu;Zhu, Hui;Dong, Zhi-Bing [Synthetic Communications,2017,vol. 47,# 16,p. 1434 - 1440] Location in patent:supporting information