Hydrochloric Acid → HCID 178484084, Verbindung

HRID 1063633Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1063633
C(O[C:6]([N:8]([CH2:10][C@H:11]1[CH2:16][CH2:15][C@H:14]([C:17]([OH:19])=[O:18])[CH2:13][CH2:12]1)C)=O)(C)(C)C.[ClH:20]>O1CCOCC1>[CH3:6][NH:8][CH2:10][C@H:11]1[CH2:16][CH2:15][C@H:14]([C:17]([OH:19])=[O:18])[CH2:13][CH2:12]1.[ClH:20]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 178484087HCID 178484087, Verbindung

Produkt 1

HCID 178484084HCID 178484084, VerbindungAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel2×

Reaktionsbedingungen

Temperatur
10 °C

Versuchsvorschrift

A solution of 3.86 g (14.23 mmol) of trans-4-[(tert-butoxycarbonyl-methyl-amino)-methyl]-cyclohexanecarboxylic acid was dissolved in 36 mL of dioxane, cooled to 10° C. and treated with 35.5 mL (142.25 mmol, 10 eq) of 4M HCl in dioxane, then warmed to RT. The solution was evaporated after 2 h to ca. 15 mL, cooled to 0° C. and precipitated with ˜100 mL of Et2O. The solid precipitate was filtrated, washed with Et2O (×3) and dried under reduced pressure to yield 2.66 g (90%) of trans-4-methylaminomethyl-cyclohexanecarboxylic acid·HCl, MS: 172 (MH+), MP: 261° C.

Aufarbeitung

  1. temperaturewarmed to RT
  2. customThe solution was evaporated after 2 h to ca. 15 mL
  3. temperaturecooled to 0° C.
  4. customprecipitated with ˜100 mL of Et2O
  5. filtrationThe solid precipitate was filtrated
  6. washwashed with Et2O (×3)
  7. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-722dd26f537f41d2aafc684d8c6dd997
Quelldatensatz
uspto-grants-2005_11
Patentnummer
US06965048B2

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