Hydrochloric Acid → Morpholine-4-carboxylic acid [1-(4-cyano-piperidin-4-ylcarbamoyl)-2-cyclohexyl-ethyl]-amide hydrochloride

HRID 1609992Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1609992
C(OC([N:8]1[CH2:13][CH2:12][C:11]([C:34]#[N:35])([NH:14][C:15](=[O:33])[CH:16]([NH:24][C:25]([N:27]2[CH2:32][CH2:31][O:30][CH2:29][CH2:28]2)=[O:26])[CH2:17][CH:18]2[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]2)[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:36]>O1CCOCC1>[ClH:36].[C:34]([C:11]1([NH:14][C:15]([CH:16]([NH:24][C:25]([N:27]2[CH2:32][CH2:31][O:30][CH2:29][CH2:28]2)=[O:26])[CH2:17][CH:18]2[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23]2)=[O:33])[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1)#[N:35]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 694173464-Cyano-4-{3-cyclohexyl-2-[(morpholine-4-carbonyl)-amino]-propionylamino}-piperidine-1-carboxylic acid t-butyl ester

Produkt 1

HCID 22260409Morpholine-4-carboxylic acid [1-(4-cyano-piperidin-4-ylcarbamoyl)-2-cyclohexyl-ethyl]-amide hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

4-Cyano-4-{3-cyclohexyl-2-[(morpholine-4-carbonyl)-amino]-propionylamino}-piperidine-1-carboxylic acid t-butyl ester (1000 mg, 2.03 mmol) was dissolved in 20 mL of 4 M HCl in dioxane and stirred for 1 hour at which time the volatiles were remove in vacuo. The resulting residue was triturated with 100 mL of diethyl ether and the resulting solid was collected by filtration under inert atmosphere (the solid is very hygroscopic) and washed 2×50 mL of diethyl ether and dried in vacuo to yield the title compound as a bright white powder (802 mg); MS, m/z 392, M−35).

Aufarbeitung

  1. customwere remove in vacuo
  2. customThe resulting residue was triturated with 100 mL of diethyl ether
  3. filtrationthe resulting solid was collected by filtration under inert atmosphere (the solid
  4. washwashed 2×50 mL of diethyl ether
  5. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-9b860294e8cd467b855278c4230bdbec
Quelldatensatz
uspto-grants-2006_01
Patentnummer
US06982272B2

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