Trifluoroacetic acid → HCID 178486747, Verbindung

HRID 228957

Reaktionsgleichung

Reaktionsgleichung von HRID 228957
FC(F)(F)C(O)=O.[CH3:8][O:9][C:10]1[CH:11]=[C:12]2[C:17](=[CH:18][C:19]=1[O:20][CH2:21][CH2:22][NH:23][C:24]([NH:33]C(OC(C)(C)C)=O)=[N:25]C(OC(C)(C)C)=O)[N:16]=[CH:15][CH:14]=[C:13]2[O:41][C:42]1[C:43]([CH3:52])=[N:44][C:45]2[C:50]([CH:51]=1)=[CH:49][CH:48]=[CH:47][CH:46]=2.[OH-].[Na+]>>[CH3:8][O:9][C:10]1[CH:11]=[C:12]2[C:17](=[CH:18][C:19]=1[O:20][CH2:21][CH2:22][NH:23][C:24]([NH2:33])=[NH:25])[N:16]=[CH:15][CH:14]=[C:13]2[O:41][C:42]1[C:43]([CH3:52])=[N:44][C:45]2[C:50]([CH:51]=1)=[CH:49][CH:48]=[CH:47][CH:46]=2

Komponenten

4

Edukt 3

HCID 6422Trifluoroacetic acidHCID 14798Sodium HydroxideHCID 178486746HCID 178486746, Verbindung

Produkt 1

HCID 178486747HCID 178486747, VerbindungAusbeute 100 %

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

Trifluoroacetic acid (1 ml) was added to N-{2-[6-methoxy-4-(2-methyl-quinolin-3-yloxy)-quinolin-7-yloxy]-ethyl}-N′,N″-diboc-guanidine (222 mg) at 0° C., and the mixture was then stirred at 0° C. for 2 hr. The reaction solution was made alkaline by the addition of a 1 N aqueous sodium hydroxide solution and was extracted with n-butanol. The n-butanol layer was washed with water and was then dried over anhydrous magnesium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by thin layer chromatography using chloroform-methanol to give the title compound (150 mg, yield 100%).

Aufarbeitung

  1. extractionwas extracted with n-butanol
  2. washThe n-butanol layer was washed with water
  3. dry with materialwas then dried over anhydrous magnesium sulfate
  4. customThe solvent was removed by distillation under the reduced pressure
  5. customthe residue was purified by thin layer chromatography

Quellen und Nachweise

ORD-Eintrag
ord-1473569bef484c709de4853e270842aa
Quelldatensatz
uspto-grants-2009_07
Patentnummer
US07560558B2

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