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Water → t-butyl [N-(t-butoxycarbonyl)-N-(methoxycarbonyl)aminomethyl]-3-nitrobenzoate

HRID 2186052
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2186052
BrC[C:3]1[CH:15]=[CH:14][C:6]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])=[CH:5][C:4]=1[N+:16]([O-:18])=[O:17].[NH:19]([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[C:20]([O:22][CH3:23])=[O:21].[K].O.[CH3:33]N(C=O)C>>[C:27]([O:26][C:24]([N:19]([CH2:33][C:5]1[C:4]([N+:16]([O-:18])=[O:17])=[CH:3][CH:15]=[CH:14][C:6]=1[C:7]([O:9][C:10]([CH3:11])([CH3:12])[CH3:13])=[O:8])[C:20]([O:22][CH3:23])=[O:21])=[O:25])([CH3:30])([CH3:29])[CH3:28]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 4

HCID 962WaterHCID 6228Dimethylformamide2×HCID 18462578t-Butyl 4-bromomethyl-3-nitrobenzoateHCID 86754983Potassium t-butyl methyl iminodicarboxylate

Produkt 1

HCID 86758139t-butyl [N-(t-butoxycarbonyl)-N-(methoxycarbonyl)aminomethyl]-3-nitrobenzoateAusbeute 73 %

Versuchsvorschrift

To a solution of t-butyl 4-bromomethyl-3-nitrobenzoate (2.27 g, 7.2 mmol) (Int. J. Peptide Res., 36, 31 (1990)) in DMF (25 mL) was added a suspension of potassium t-butyl methyl iminodicarboxylate (J.C.S. Perkin I, 1088, (1977)) (1.56 g, 7.3 mmol) in DMF (20 mL). The dark brown solution was stirred 1 h and poured into water and extracted with ethyl acetate. The combined organic layers were washed with water, dried (sodium sulfate) and concentrated to give a pale orange oil which was purified by flash chromatography (silica gel, 20% ethyl acetate/hexane) to give the title compound (2.15 g, 73%). 1H NMR (400 MHz, CDCl3) δ8.65 (s, 1H), 8.2 (d, 1H), 7.45 (d, 1H), 5.3 (s, 2H), 3.8 (s, 3H), 1.6 (s, 9H), 1.45 (s, 9H).

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. washThe combined organic layers were washed with water
  3. dry with materialdried (sodium sulfate)
  4. concentrationconcentrated
  5. customto give a pale orange oil which
  6. customwas purified by flash chromatography (silica gel, 20% ethyl acetate/hexane)

Quellen und Nachweise

ORD-Eintrag
ord-c948812f004c4f168421cb9f6ffe02d7
Quelldatensatz
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06403578B1

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