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1-Hydroxybenzotriazole → 3-({[N-(t-butoxycarbonyl)-O-ethyl-N-methyl-3-oxoseryl]amino}methyl)-5-methyl-1,2-oxazole

HRID 1519681
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1519681
[C:1]([O:5][C:6]([N:8]([CH3:18])[C@H:9]([C:15]([OH:17])=O)[C:10](=[O:14])[O:11][CH2:12][CH3:13])=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH3:19][C:20]1[O:24][N:23]=[C:22]([CH2:25][NH2:26])[CH:21]=1.CCN=C=NCCCN(C)C.Cl.C1C=CC2N(O)N=NC=2C=1.C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl.O>[C:1]([O:5][C:6]([N:8]([CH3:18])[C@H:9]([C:15]([NH:26][CH2:25][C:22]1[CH:21]=[C:20]([CH3:19])[O:24][N:23]=1)=[O:17])[C:10](=[O:14])[O:11][CH2:12][CH3:13])=[O:7])([CH3:2])([CH3:3])[CH3:4]
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Komponenten

8

Edukt 5

HCID 757711-HydroxybenzotriazoleHCID 516892Sodium BicarbonateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27763061-(5-Methyl-1,2-oxazol-3-yl)methanamineHCID 86679248N-(t-butoxycarbonyl)-O-ethyl-N-methyl-3-oxoserine2×

Produkt 1

HCID 71268225
3-({[N-(t-butoxycarbonyl)-O-ethyl-N-methyl-3-oxoseryl]amino}methyl)-5-methyl-1,2-oxazole
Ausbeute 67,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6212ChloroformLösungsmittel

Versuchsvorschrift

N-(t-butoxycarbonyl)-O-ethyl-N-methyl-3-oxoserine (Intermediate 7-1, 2.3 g), 1-(5-methyl-1,2-oxazol-3-yl)methanamine (1.0 g), WSC.HCl (2.4 g), HOBt.H2O (1.9 g), and chloroform (24 mL) were stirred overnight at room temperature. A saturated aqueous solution of sodium hydrogen carbonate was added to the reaction mixture, and the mixture was extracted with chloroform. The extract was dried over anhydrous magnesium sulfate, and the desiccant was filtered out. Then, the solvent was distilled off under reduced pressure, and the resulting residue was purified by OH type silica gel column chromatography (gradient elution with chloroform/methanol=98/2→92/8) to obtain 3-({[N-(t-butoxycarbonyl)-O-ethyl-N-methyl-3-oxoseryl]amino}methyl)-5-methyl-1,2-oxazole (pale yellow oil) (2.1 g, 67%).

Aufarbeitung

  1. extractionthe mixture was extracted with chloroform
  2. dry with materialThe extract was dried over anhydrous magnesium sulfate
  3. filtrationthe desiccant was filtered out
  4. distillationThen, the solvent was distilled off under reduced pressure
  5. customthe resulting residue was purified by OH type silica gel column chromatography (gradient elution with chloroform/methanol=98/2→92/8)

Quellen und Nachweise

ORD-Eintrag
ord-45c83e20d2754f20970fbf900c7a05b2
Quelldatensatz
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09073821B2

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