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Carbon tetrabromide → 1,4-Bis(t-butoxycarbonyl)-2-(2-bromoethyl)piperazine

HRID 352834
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 352834
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:10][CH:9]1[CH2:21][CH2:22]O)=[O:7])([CH3:4])([CH3:3])[CH3:2].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Br)(Br)(Br)[Br:44]>C(Cl)Cl>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:10][CH:9]1[CH2:21][CH2:22][Br:44])=[O:7])([CH3:4])([CH3:3])[CH3:2]
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Komponenten

5

Edukt 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 22710988di-tert-Butyl 2-(2-hydroxyethyl)piperazine-1,4-dicarboxylate

Produkt 1

HCID 227107281,4-Bis(t-butoxycarbonyl)-2-(2-bromoethyl)piperazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

In methylene chloride (70 ml) were dissolved 1,4-bis(tert-butoxycarbonyl)-2-(2-hydroxyethyl)piperazine (2.01 g) and triphenylphosphine (1.98 g). Under ice cooling, carbon tetrabromide (3.07 g) was added to the resulting solution, followed by stirring at room temperature for 2.5 hours. The reaction mixture was extracted with a 10% aqueous solution of sodium thiosulfate. The organic layer was washed with saturated aqueous NaCl solution, dried over anhydrous sodium sulfate an distilled under reduced pressure to remove the solvent. The residue was subjected to column chromatography (hexane:ethyl acetate=4:1) using as a carrier silica gel, whereby the title compound (2.20 g) was obtained as colorless powder.

Aufarbeitung

  1. extractionThe reaction mixture was extracted with a 10% aqueous solution of sodium thiosulfate
  2. washThe organic layer was washed with saturated aqueous NaCl solution
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationan distilled under reduced pressure
  5. customto remove the solvent
  6. customwas obtained as colorless powder

Quellen und Nachweise

ORD-Eintrag
ord-39831b8d51d94294b2ce91658b8f3627
Quelldatensatz
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06747023B1

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