Organo-phosphorus compounds S 0080The First Synthesis of Diethyl α,α-Chlorofluorobenzylphosphonates. -The title compounds (III) are prepared from α-hydroxyphosphonates by chlorination followed by fluorination. -(WU, D.; HE, Y.; TANG, R.; GUAN*
A simple preparation of ethyl 2,5‐dimethylfuran‐3‐carboxylate (3), 2,5‐dimethylfuran‐3,4‐dicarboxylic acid (4), and diethyl 2,5‐dimethylfuran‐3,4‐dicarboxylate (5) by treatment of diethyl 2,3‐diacetylsuccinate (2) with aqueous HCl is reported. The reaction is performed under organic solvent free conditions from a readily available cheap starting material. J. Heterocyclic Chem., (2009).
Furan derivatives R 0060A Simple Preparation of Ethyl 2,5-Dimethylfuran-3-carboxylate and 2,5-Dimethylfuran-3,4-dicarboxylic Acid from Diethyl 2,3-Diacetylsuccinate. -The products can be easily prepared by thermal or microwave-promoted Paal-Knorr cyclization. The outcome of the reaction can be simply influenced by adjusting the HCl concentration. Diester (II) is only obtained under microwave irradiation.
Starting from a-hydroxyphosphonates, a wide variety of diethyl a,a-chlorofluorobenzylphosphonates have been obtained in pure form in a two-step procedure. The first step was chlorination of a-hydroxyphosphonates with Ph 3 P and CCl 4 , while the second step was fluorination with N-fluorobisbenzenesulfonimide.
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