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MS ont été effectuées sur un appareil HP équipé d'une colonne capillaire Chrompack (Cpsil525, 25 m x 0,32 mm, df = 0,11 µm) ,
Chemstation équipée d'une colonne 300 mm x 7,5 mm PLgel Mixed-D 5 µm/10 4 Å, d'un détecteur UV-Visible à barette de diode calée à 420 nm et d'un détecteur d'indice de réfraction. La température de la colonne est maintenue à 40 °C et le débit à 1 mL.min -1 . La calibration de la colonne est obtenue à partir d'échantillons de polystyrène (PS) monodisperse (PS) (S-M2-10*, polymer Laboratories), 1100. ,
21 mol) sont introduits en solution dans 120 mL d'acide acétique et 100 mL d'eau. 5,7 équivalents de zinc (78 g, 1,19 mol) sont ajoutés petit à petit sous forme de poudre dans le milieu. La température est portée à 120 °C pour activer la réaction. Le milieu est laissé 24 heures à 120 °C puis filtré sur celite et extrait à l'hexane, Les phases organiques sont lavées au NaHCO 3 , avec de l'eau et une solution saturée de NaCl puis séchées sur Na 2 SO 4 . Le produit brut est composé à 98, pp.5-8 ,
RMN 13 C (CDCl 3 ) : 142,6, EIMS m/z (intensité relative) : 178 (M ·+, pp.9522-71 ,
9 mmol) sont introduits en solution dans 8 mL d'acide acétique et 5 mL d'eau. 10 équivalents de zinc (11,45 g, 0,17 mol) sont ajoutés petit à petit sous forme de poudre dans le milieu. La température est portée à 120 °C pour activer la réaction. Le milieu est laissé pendant 24 heures à 120 °C puis filtré sur celite et extrait à l'hexane, Les phases organiques sont lavées au NaHCO 3 , avec de l'eau et une solution saturée de NaCl puis séchées sur Na 2 SO 4 . Le produit brut est purifié sur HPLC (éluant : acétonitrile). 2,7 g de produit sont obtenus, pp.5-8 ,
mmol) sont introduits en solution dans 20 mL d'éther diéthylique anhydre à -78 °C, pp.5-8 ,
RMN 13 C (CDCl 3 ) : ? = 147,3, pp.616127-616158 ,
ambiante (~1h30) puis le milieu est mis au reflux du THF toute la nuit. Le milieu est hydrolysé. Le précipité marron, très difficile à filtrer, peut être solubilisé par légère acidification du milieu avec de l'acide chlorhydrique 1,5 M ,
7 Hz) RMN 13 C (CDCl 3 ): 155,8, pp.88158453-188, 2009. ,