StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Lithium hydroxide, monohydrate → 2-{4-[((3R,5S)-4-{[(1,1-Dimethylethyl)oxy]carbonyl}-3,5-dimethyl-1-piperazinyl)methyl]phenyl}-2-methylpropanoic Acid

HRID 43355
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 43355
[CH3:1][C:2]([C:8]1[CH:13]=[CH:12][C:11]([CH2:14][N:15]2[CH2:20][C@H:19]([CH3:21])[N:18]([C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23])[C@H:17]([CH3:29])[CH2:16]2)=[CH:10][CH:9]=1)([CH3:7])[C:3]([O:5]C)=[O:4].O.[OH-].[Li+]>O.O1CCOCC1>[CH3:28][C:25]([O:24][C:22]([N:18]1[C@@H:17]([CH3:29])[CH2:16][N:15]([CH2:14][C:11]2[CH:12]=[CH:13][C:8]([C:2]([CH3:1])([CH3:7])[C:3]([OH:5])=[O:4])=[CH:9][CH:10]=2)[CH2:20][C@H:19]1[CH3:21])=[O:23])([CH3:26])[CH3:27]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 168937Lithium hydroxide, monohydrateHCID 252242061,1-Dimethylethyl (2R,6S)-4-({4-[1,1-dimethyl-2-(methyloxy)-2-oxoethyl]phenyl}methyl)-2,6-dimethyl-1-piperazinecarboxylate

Produkt 1

HCID 252242082-{4-[((3R,5S)-4-{[(1,1-Dimethylethyl)oxy]carbonyl}-3,5-dimethyl-1-piperazinyl)methyl]phenyl}-2-methylpropanoic AcidAusbeute 82,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962Water
Lösungsmittel
HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A mixture of D47 (395 mg, 0.978 mmol) and lithium hydroxide monohydrate (82 mg, 1.95 mmol) in water (5 ml) and 1,4-dioxane (10 ml) was stirred at room temperature for 3 days. The solvents were removed in vacuo and the residue dissolved in water. The solution was washed with ether, acidified to pH4 with 1M HCl then extracted with DCM (×2). The combined organics were dried (Na2SO4) and concentrated in vacuo to give the title compound as a yellow foam (316 mg). δH (CDCl3, 250 MHz) 7.35 (4H, m), 4.11 (2H, br), 3.71 (2H, br), 2.67 (2H, br), 2.17 (2H, br), 1.61 (6H, s), 1.46 (9H, s), 1.33 (6H, br d). MS (ES): MH+ 391, (M−H+) 389.

Aufarbeitung

  1. customThe solvents were removed in vacuo
  2. dissolutionthe residue dissolved in water
  3. washThe solution was washed with ether
  4. extractionthen extracted with DCM (×2)
  5. dry with materialThe combined organics were dried (Na2SO4)
  6. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-52225b07782d452db6fd71c6a69065ae
Quelldatensatz
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08536182B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion