Nucleating agent intermediate 2,2′-methylene-bis­(4,6-di-tert-butylphenol) phosphate chloride was synthesized successfully in a continuous flow by the phosphorylation reaction for the first time. After evaluating several different continuous flow reactors, the continuous Coflore agitated cell reactor (ACR) designed based on the continuous stirred-tank reactor (CSTR) principle was proved capable of overcoming the severe channel clogging caused by the precipitation product triethylamine hydrochloride. This can be attributed to the violent agitation and particle size control by the moving agitators. The yield in continuous flow after optimization reached nearly 98% at 100 °C within the residence time of only 4 min and the optimal equivalents of triethylamine and POCl3 are 2.8 and 1.1, respectively. In contrast to the batch operation, the yield has been increased through continuous operation. This is an effective method for the synthesis of the desired product and exhibits the merits of short residence time, easy operation, and straightforward scale-up.

A convenient procedure for the catalytic hydrosilylation of secondary anilides bearing an oxazolyl group has been developed. In the presence of inexpensive NiBr 2 , the reduction of functionalized secondary amides with nontoxic and air-stable TMDS proceeded smoothly to give the corresponding functionalized amines. The method displays a broad applicability for the reduction of many types of substrates, and shows good compatibility and excellent chemoselectivity for several sensitive functional groups such as halo, ester and nitro groups.[a] J.

A practical approach to the synthesis of antioxidant 4,4′-dicumyldiphenylamine (DCDPA) and its derivatives by Friedel−Crafts alkylation of aromatic amines was developed under continuous flow conditions. Because of the enhanced mass and heat transfer features of the microreactor, the reaction time was significantly reduced in contrast to a batch mode. The reaction was carried out using a 1:6 v/v ethanol/Cl(CH 2 ) 2 Cl cosolvent system with ZnCl 2 as the catalyst to achieve satisfactory yields. This is an effective method for the synthesis of DCDPA and its derivatives with excellent para selectivity that has the merits of shorter reaction time, easy operation, and straightforward scale-up.

Metrics & MoreArticle RecommendationsI n the published article, Scheme 2 contained an error. The corrected scheme is given here.