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Ammonia → HCID 57588245, Verbindung

HRID 2194621
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2194621
CC1C=CC(S(O[CH2:12][C@@H:13]2[CH2:18][CH2:17][N:16]([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH2:15][C@H:14]2[O:26][CH3:27])(=O)=O)=CC=1.[NH3:28]>C1COCC1>[NH2:28][CH2:12][C@@H:13]1[CH2:18][CH2:17][N:16]([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH2:15][C@H:14]1[O:26][CH3:27]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 222AmmoniaHCID 57588246HCID 57588246, Verbindung

Produkt 1

HCID 57588245HCID 57588245, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A mixture of intermediate (49) (0.065 mol) in THF (250 ml) was treated with liquid NH3 in an autoclave at 125° C. during 16 hours. The reaction mixture was filtered and the filtrate was evaporated. The residue was partitioned between a 5% aqueous NaOH solution and DCM. The organic layer was separated, dried, filtered and the solvent was evaporated, yielding 16 g of 1,1-dimethylethyl(trans)-4-(aminomethyl)-3-methoxy-1-piperidinecarboxylate (intermediate (50).

Aufarbeitung

  1. filtrationThe reaction mixture was filtered
  2. customthe filtrate was evaporated
  3. customThe residue was partitioned between a 5% aqueous NaOH solution and DCM
  4. customThe organic layer was separated
  5. customdried
  6. filtrationfiltered
  7. customthe solvent was evaporated

Quellen und Nachweise

ORD-Eintrag
ord-b9ef62f1e0fa417a88608f0ab82cc92c
Quelldatensatz
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08334304B2

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