Sodium Bicarbonate → HCID 21941354, Verbindung

HRID 1158850Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1158850
F[B-](F)(F)F.C[O+:7]([CH3:9])[CH3:8].[N+:10]([C:13]1[CH:29]=[CH:28][C:16]([CH2:17][O:18][C:19]([N:21]2C[CH2:25][NH:24][C:23](=O)[CH2:22]2)=[O:20])=[CH:15][CH:14]=1)([O-:12])=[O:11].C(=O)([O-])O.[Na+]>ClCCl>[CH3:8][O:7][CH:9]1[CH2:25][NH:24][CH2:23][CH2:22][N:21]1[C:19]([O:18][CH2:17][C:16]1[CH:15]=[CH:14][C:13]([N+:10]([O-:12])=[O:11])=[CH:29][CH:28]=1)=[O:20]

Komponenten

5

Edukt 3

HCID 516892Sodium BicarbonateHCID 2735153Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1)HCID 21941454(4-Nitrophenyl)methyl 3-oxo-1-piperazinecarboxylate

Produkt 1

HCID 21941354HCID 21941354, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Trimethyloxonium tetrafluoroborate (97%, 3.7 g) was added to the dry dichloromethane (120 mL) solution of 4-p-nitrobenzyloxycarbonyl-2-oxopiperazine (6.7 g) at room temperature and stirred for 17 hours. The reaction mixture was treated with saturated sodium hydrogen carbonate aqueous solution, and the organic layer was separated. The aqueous layer was extracted with ethyl acetate (3×100 mL), then the combined organic layer was washed with saturated sodium hydrogen carbonate aqueous solution and brine. The organic layer was dried (MgSO4) and filtered. The filtrate was concentrated under reduce pressure and the title compound was obtained as a pale brown solid. Yield; 5.7 g, 80.6.

Aufarbeitung

  1. customthe organic layer was separated
  2. extractionThe aqueous layer was extracted with ethyl acetate (3×100 mL)
  3. washthe combined organic layer was washed with saturated sodium hydrogen carbonate aqueous solution and brine
  4. dry with materialThe organic layer was dried (MgSO4)
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-4681d1050260473ab4cb4df3e68951ae
Quelldatensatz
uspto-grants-2010_10
Patentnummer
US07812014B2

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