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

Sulfuric acid magnesium salt (1:1) → Fingolimod Impurity 4

HRID 635461
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 635461
[Li].[C:2]([NH:5][CH:6]([CH2:11][CH2:12][C:13]1[CH:18]=[CH:17][C:16]([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])=[CH:15][CH:14]=1)[C:7](OC)=[O:8])(=[O:4])[CH3:3].S([O-])([O-])(=O)=O.[Mg+2]>O1CCCC1>[C:2]([NH:5][CH:6]([CH2:11][CH2:12][C:13]1[CH:18]=[CH:17][C:16]([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])=[CH:15][CH:14]=1)[CH2:7][OH:8])(=[O:4])[CH3:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 3028194LithiumHCID 22618836Methyl 2-acetamido-4-(4-octylphenyl)butyrate

Produkt 1

HCID 22618882Fingolimod Impurity 4Ausbeute 65,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel3×

Versuchsvorschrift

To a suspension of lithium abluminum hydride (1.2 g) in tetrahydrofuran (100 ml), a solution of methyl 2-acetamido-4-(4-octylphenyl)butyrate (11 g) in tetrahydrofuran (200 ml) was added and the suspension was stirred at room temperature for 30 minutes. An aqueous tetrahydrofuran (70%, 10 ml) was added to the solution and the mixture was left standing overnight. Magnesium sulfate was added to the mixture, the precipitate was filtered off and the solvent was distilled away under reduced pressure. The residue was dissolved in ethyl acetate, the solution was washed with a dilute hydrochloric acid, an aqueous sodium hydrogencarbonate solution and a saturated brine in order and dried over sodium sulfate. The solvent was distilled away under reduced pressure to give the subject compound (6.6 g). MS: 319(M+).

Aufarbeitung

  1. waitthe mixture was left
  2. waitstanding overnight
  3. filtrationthe precipitate was filtered off
  4. distillationthe solvent was distilled away under reduced pressure
  5. dissolutionThe residue was dissolved in ethyl acetate
  6. washthe solution was washed with a dilute hydrochloric acid
  7. dry with materialan aqueous sodium hydrogencarbonate solution and a saturated brine in order and dried over sodium sulfate
  8. distillationThe solvent was distilled away under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-006b48c970d24ca28ebe3a94d9efdfa0
Quelldatensatz
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06187821B1

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion