Pyridine → tert-Butyl 3-carbamoylmorpholine-4-carboxylate

HRID 1351345

Reaktionsgleichung

Reaktionsgleichung von HRID 1351345
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][O:11][CH2:10][CH:9]1[C:14]([OH:16])=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].[N:17]1C=CC=CC=1.C(OC(OC(C)(C)C)=O)(OC(C)(C)C)=O>O1CCOCC1>[NH2:17][C:14]([CH:9]1[CH2:10][O:11][CH2:12][CH2:13][N:8]1[C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:7])=[O:16]

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 90495Di-tert-butyl dicarbonateHCID 27601334-(tert-Butoxycarbonyl)morpholine-3-carboxylic acid

Produkt 1

HCID 21098189tert-Butyl 3-carbamoylmorpholine-4-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

To a stirred solution of the compound prepared in Step 1 (1 eq.), pyridine (0.6 eq.) and di-t-butyl dicarbonate (1.3 eq.) in dioxane (0.6 M), NH4HCO3 (1.26 eq.) was added and the mixture was stirred at room temperature for 20 hours. Mixture was concentrated, taken up in EtOAc and washed with water and brine. Organics were dried over Na2SO4 and evaporated giving the title product as an oil which crystallized at room temperature.

Aufarbeitung

  1. concentrationMixture was concentrated
  2. washwashed with water and brine
  3. dry with materialOrganics were dried over Na2SO4
  4. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-f2efb6265014408f8e189eb547b261b0
Quelldatensatz
uspto-grants-2007_05
Patentnummer
US07217713B2

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