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, Les ligands L11 et L12 ? Acide 6-(pyrrol-1-yl)-hexanoïque : 13,12 g d'acide 6-amino-hexanoïque (100 mmol) sont dissous dans 13 mL de 2,5-diméthoxytétrahydrofuranne (100 mmol) et 100 mL d'une solution aqueuse eau/acide acétique (60/40) Le milieu réactionnel est porté à 70 °C pendant 2 h 30. La phase aqueuse est acidifiée jusqu'à pH 3 avec de l'acide chlorhydrique concentré puis extraite avec du dichlorométhane
, eau glacée, on ajoute successivement 26,32 g de chlorure de tosyle (138,1 mmol) et une solution de 5,72 g de 6-(pyrrol-1-yl)-hexan-1-ol (34,2 mmol) dans 150 mL de pyridine sous agitation Après 3 h, le milieu réactionnel est placé toute une nuit à 4 °C sans agitation. On note l'apparition d'un précipité noir que l'on dissout dans de l'eau. Cette phase aqueuse est extraite avec du diéthyl-éther. La phase organique est lavée avec une solution aqueuse d'acide chlorhydrique à 5 % en volume, puis à l'eau et ensuite séchée sur Na 2 SO 4 . Le solvant est évaporé sous vide. On obtient alors 9
, 68 g de 1-tosyl-6-(pyrrol-1-yl)-hexane (30,1 mmol), on ajoute 60 mL d'une solution saturée en KBr ainsi que 562 mg de dibenzo, pp.18-24
, 15 mL de THF anhydre et 12 mL de n-butyl-lithium à 2,5 M dans l'hexane (30 mmol) On procède alors à l'addition goutte à goutte d'une solution de 5,01 g de dmbpy (27,2 mmol) dans 200 mL de THF anhydre. On laisse sous agitation 1 h à -50 °C. Puis on ajoute 6,18 g de 6-bromo-(pyrrol-1-yl)hexane dans 10 mL de THF anhydre. Après une nuit, on hydrolyse avec 100 mL d'eau à température ambiante. La phase aqueuse est extraite avec du diéthyl-ether On obtient 1, p.30
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