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catalyseur de formule k₅pw₁₁cro₃₉n₃.
catalyst having the formula k₅pw₁₁cro₃₉n₃.
Son Güncelleme: 2014-12-04
Kullanım Sıklığı: 2
Kalite:
analyses : spectre x h rmn : dmso d s δ (ppm) l,83(d), 3,03 (m) : 2h ; 2, 79 (s) : ch3-n ; 3 , 13 (m) , 3,42 (masqué) : 2h ; 3 , 26 (masqué) , 3, 36 (masqué) : 2h ; 3,54(d) : lh(axial) ; 4,13 (s) : 1h (équatorial) ; 6,35(s) : 1h ; 6,73(s) : 1h ; 7,62(s) : 1h ; 9,37(sl), ll,31(sl), 12,9(s) : 3h (mobiles). exemple 3 : trifluoroacétate de 5 , 7-dihydroxy-8- [ (3s, 4r) -3 - hydroxy-l-méthyl-4-piperidinyl] -2- (5-méthyl-3-isoxazolyl) -4h- benzopyran-4-one stade a) : 5, 7-diméthoxy-8- [ (3s, 4r) -3 -hydroxy-l-méthyl-4 - piperidinyl] -2- (5-méthyl-3 -isoxazolyl) -4h-benzopyran-4-one 1) condensation : 1- [2-hydroxy-4, 6-diméthoxy-3 - [ (3s, 4r) -3- hydroxy-1-méthyl -4 -piperidinyl] phényl] -3- (5-méthyl-3- isoxazolyl ) 1 , 3 -propanedione dans un ballon de 30 cm3 , sous n2 , on introduit 310 mg de nah à 50 % dans l'huile (m=24) (6.5 mmol-4eq.), 10 cm3 de thf anhydre, 500 mg d ' acétoflocinopipéridol (1.6 mmol) par fractions, 2 gouttes d ' etoh et 12 mg de dibenzo-18-cro n-6 (m=360.41) (0.03 mmol-2 % molaire).
[0193] analyses: [0194] 1 h nmr spectrum: dmso d 6 δ (ppm) 1.83(d), 3.03(m): 2h; 2.79(s): ch3-n; 3.13(m), 3.42(masked): 2h; 3.26(masked), 3.36(masked): 2h; 3.54(d): 1h(axial); 4.13(s): 1h(equatorial); 6.35(s): 1h; 6.73(s): 1h; 7.62(s): 1h; 9.37(bs), 11.31(bs), 12.9(s): 3h (mobiles). example 3 5,7-dihydroxy-8-[(3s,4r)-3-hydroxy-1-methyl-4-piperidinyl]-2-(5-methyl-3-isoxazolyl)-4h-benzopyran-4-one, trifluoroacetate [0195] stage a): 5,7-dimethoxy-8-[(3s,4r)-3-hydroxy-1-methyl-4-piperidinyl]-2-(5-methyl-3-isoxazolyl)-4h-benzopyran-4-one [0196] 1) condensation: 1-[2-hydroxy-4,6-dimethoxy-3-[(3s,4r)-3-hydroxy-1-methyl-4-piperidinyl]phenyl]-3-(5-methyl-3-isoxazolyl)1,3-propanedione [0197] 310 mg of nah at 50% in oil (m=24) (6.5 mmol-4 eq.), 10 cm3 of anhydrous thf, 500 mg of acetoflocinopiperidol (1.6 mmol) by fractions, 2 drops of etoh and 12 mg of dibenzo-18-crown-6 (m=360.41) (0.03 mmol-2% molar) is introduced, under n2, into a 30 cm3 flask.
Son Güncelleme: 2014-12-03
Kullanım Sıklığı: 1
Kalite: