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Hydrogen chloride-ethyl acetate → HCID 86678702, Verbindung

HRID 1620509
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1620509
[OH:1][CH2:2][CH:3]1[CH2:10][CH:9]2[CH2:11][CH:5]([CH2:6][N:7](C(OC(C)(C)C)=O)[CH2:8]2)[CH2:4]1.[ClH:19].C(OCC)(=O)C>CO>[ClH:19].[CH:9]12[CH2:11][CH:5]([CH2:4][CH:3]([CH2:2][OH:1])[CH2:10]1)[CH2:6][NH:7][CH2:8]2
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 86678701HCID 86678701, Verbindung

Produkt 1

HCID 86678702HCID 86678702, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of 3-tert-butyl 7-hydroxymethyl-3-azabicyclo[3.3.1]nonane-3-carboxylate (7.78 g) in methanol (76 mL) was added 4M hydrogen chloride/ethyl acetate solution (76 mL). The reaction mixture was stirred at room temperature for 4 hr, and the solvent was evaporated under reduced pressure. The residue was dissolved in methanol (50 mL), and Amberlyst A-21 was added. The mixture was stirred at room temperature for 20 min, and the solid was removed by filtration. The solvent was evaporated under reduced pressure, and the residue was recrystallized from ethanol/ethyl acetate to give the title compound (5.22 g).

Aufarbeitung

  1. customthe solvent was evaporated under reduced pressure
  2. dissolutionThe residue was dissolved in methanol (50 mL)
  3. additionAmberlyst A-21 was added
  4. stirringThe mixture was stirred at room temperature for 20 min
  5. customthe solid was removed by filtration
  6. customThe solvent was evaporated under reduced pressure
  7. customthe residue was recrystallized from ethanol/ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-189db74387ae42bab70b3163274221e0
Quelldatensatz
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08772277B2

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