Hydrochloric Acid → HCID 71079543, Verbindung

HRID 337213Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 337213
C(OC(=O)[NH:7][CH:8]1[CH2:13][CH2:12][N:11]([S:14]([C:17]2[CH:22]=[CH:21][C:20]([N:23]([CH3:32])[C:24]([CH:26]3[CH2:31][CH2:30][O:29][CH2:28][CH2:27]3)=[O:25])=[CH:19][CH:18]=2)(=[O:16])=[O:15])[CH2:10][CH2:9]1)(C)(C)C.Cl>O1CCOCC1>[NH2:7][CH:8]1[CH2:9][CH2:10][N:11]([S:14]([C:17]2[CH:18]=[CH:19][C:20]([N:23]([CH3:32])[C:24]([CH:26]3[CH2:31][CH2:30][O:29][CH2:28][CH2:27]3)=[O:25])=[CH:21][CH:22]=2)(=[O:15])=[O:16])[CH2:12][CH2:13]1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 71060228(1-{4-[Methyl-(tetrahydro-pyran-4-carbonyl)-amino]-benzenesulfonyl}-piperidin-4-yl)-carbamic acid tert-butyl ester

Produkt 1

HCID 71079543HCID 71079543, VerbindungAusbeute 111,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

[(1-{4-[Methyl-(tetrahydro-pyran-4-carbonyl)-amino]-benzenesulfonyl}-piperidin-4-yl)-carbamic acid tert-butyl ester (0.17 g, 0.4 mmol) was suspended in a 4M solution of HCl in Dioxane (5 ml). The resulting suspension was stirred at room temperature for 3 hours. After this time the solution was concentrated under vacuum, then azeotroped with methanol and suspended in diethyl ether. The resulting solid precipitate was then collected by filtration, washed with diethyl ether and dried under vacuum to afford the title compound (0.17 g, Quantitative yield) as a white solid. Tr=1.20 min, m/z (ES+) (M+H)+ 382.

Aufarbeitung

  1. concentrationAfter this time the solution was concentrated under vacuum
  2. customazeotroped with methanol
  3. filtrationThe resulting solid precipitate was then collected by filtration
  4. washwashed with diethyl ether
  5. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-a26f90ed91a547dd8607b918e78f18dc
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08889716B2

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