Triethylamine → tert-Butyl 3-cyanomorpholine-4-carboxylate

HRID 1161900Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1161900
[NH2:1][C:2]([CH:4]1[CH2:9][O:8][CH2:7][CH2:6][N:5]1[C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])=O.C(N(CC)CC)C.FC(F)(F)C(OC(=O)C(F)(F)F)=O>C(Cl)Cl>[C:2]([CH:4]1[CH2:9][O:8][CH2:7][CH2:6][N:5]1[C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])#[N:1]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 9845Trifluoroacetic anhydrideHCID 21098189tert-Butyl 3-carbamoylmorpholine-4-carboxylate

Produkt 1

HCID 21098190tert-Butyl 3-cyanomorpholine-4-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A solution of the product of Step 2 (1 eq.) and triethylamine (2.1 eq.) in CH2Cl2 (0.1 M) was cooled to 0° C. and trifluoroacetic anhydride (1.1 eq.) added dropwise under nitrogen. Stirring was continued 3.5 hours more at room temperature and volatiles removed in vacuo. Residues taken in EtOAc were washed with water, brine and dried over Na2SO4. Evaporation gave the title compound as a brown solid.

Aufarbeitung

  1. customvolatiles removed in vacuo
  2. washwere washed with water, brine
  3. dry with materialdried over Na2SO4
  4. customEvaporation

Quellen und Nachweise

ORD-Eintrag
ord-73503a154c2c4edaa8da2ca3f50fc988
Quelldatensatz
uspto-grants-2010_10
Patentnummer
US07820660B2

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