On filtre le précipité que l'on lave au cyclohexane et à l'éther. On obtient un solide beige avec un rendement de 76% ,
1 g, 1 eq) est mis en solution dans 13 ml de BuOH. A cette solution on rajoute la benzylamine (4.45 mmol, 0.6 ml, 1.2 eq) et la Et 3 N (18.5 mmol, 2.6 ml, 5 eq) Après chauffage à reflux pendant 20 h, un solide se forme. Ce dernier est filtré, lavé avec 1 ml de BuOH froid et séché à l'étuve. La réaction est suivie par plaque CCM (DCM/ Cyc, On obtient un solide jaune clair avec un Rdt 97% ,
on dissout le produit 33d (3.28 mmol, 1.2 g, 1 eq) dans 65 ml de dichlorométhane, puis on additionne 0,88 g (1.5 eq) d'acide meta-chloroperbenzoïque a 80% ,
on dissout le produit 33e (3.8 mmol, 1g, 1 eq) dans 65 ml de dichlorométhane, puis on additionne 0,78 g (1.5 eq) d'acide meta-chloroperbenzoïque a 80% ,
le produit 38d (1 mmol, 0.4 g, 1 eq) est mis en réaction avec du Raminobutanol (8 mmol, 0.75 ml, 8 eq) en chauffant à 100°C pendant 24 h. Après extraction par DCM et évaporation sous vide ,
On obtient une poudre crème avec un Rdt de 35%, pp.89-95 ,
mmol, 0.4 g, 1 eq) est mis en réaction avec du 2- aminopropane-1,3-diol (5 mmol, 0.6g, 5 eq) en chauffant à 100°C pendant 12 h. après extraction par AcOEt et évaporation sous vide, le produit formé cristallisé dans l'éther, pp.38-85 ,
(ppm): 3.50 (s, 4H, 2 CH 2 OH), 3.92 (s, 1H, pp.64-67 ,
5 mmol, 0.5 g, 1 eq) est mis en réaction avec du Raminobutanol (7.5 mmol, 0.67 ml, 5 eq) en chauffant à 100°C pendant 48 h. Après extraction par DCM, on purifie le brut sur une colonne (DCM/ AcOEt, puis on évapore sous vide, le produit formé cristallise dans l'éther, p.38 ,
On obtient une poudre crème avec un Rdt de 35%, pp.110-110 ,
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