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

HRID 1161899Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1161899
[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-2f15ca6eefaa4172a740aee2f25b055d
Quelldatensatz
uspto-grants-2010_10
Patentnummer
US07820660B2

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