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SYNTHESIS AND CHARACTERIZATION OF METHYLATED TETRATHIAFULVALENES - NEW ROUTE TO THE TTF PREPARATION

H MORA,JM FABRE,L GIRAL,C MONTGINOUL

BULLETIN DES SOCIETES CHIMIQUES BELGES（1992）

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Abstract
We propose an improved general method for the synthesis of tetrathiafulvalene and its methylated derivatives. TTF is obtained in a five steps preparation offering a high Overall yield. Concerning the unsymmetrically methylated tetrathiafulvalenes, four different procedures are analysed. It is shown the best routes to prepare trimethyltetrathiafulvalene are a WTTIG type reaction, and a selective synthesis based on a WITTIG-HORNER reaction. The monomethyltetrathiafulvalene has been isolated in a 96 % state of purity.
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