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

Fumaric Acid → N-[(6R,7S)-7-(3,4-dichlorophenyl)-1,4-oxazepan-6-yl]acetamide monofumarate

HRID 1022621
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1022621
[C:1]([NH:4][C@H:5]1[C@H:11]([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([Cl:19])[CH:13]=2)[O:10][CH2:9][CH2:8][N:7](C(OC(C)(C)C)=O)[CH2:6]1)(=[O:3])[CH3:2].C(OCC)(=O)C.Cl.[C:34]([OH:41])(=[O:40])/[CH:35]=[CH:36]/[C:37]([OH:39])=[O:38]>C(O)C>[C:34]([OH:41])(=[O:40])/[CH:35]=[CH:36]/[C:37]([OH:39])=[O:38].[Cl:19][C:14]1[CH:13]=[C:12]([C@@H:11]2[O:10][CH2:9][CH2:8][NH:7][CH2:6][C@H:5]2[NH:4][C:1](=[O:3])[CH3:2])[CH:17]=[CH:16][C:15]=1[Cl:18]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 444972Fumaric AcidHCID 21866389Hydrogen chloride-ethyl acetateHCID 66975754tert-butyl (6R,7S)-6-(acetylamino)-7-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate

Produkt 1

HCID 86663854N-[(6R,7S)-7-(3,4-dichlorophenyl)-1,4-oxazepan-6-yl]acetamide monofumarateAusbeute 106,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702
Ethanol
Lösungsmittel

Versuchsvorschrift

To tert-butyl (6R,7S)-6-(acetylamino)-7-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate (200 mg) was added 4.0 M hydrogen chloride-ethyl acetate solution (4 mL), and the mixture was stirred at room temperature for 1 hr. The residue obtained by concentration under reduced pressure was desalted by a solid phase extraction resin (column: PL StrastoSphere solid phase extraction resin (PL-HCO3 MP StratoSpheres™), 500 mg, StrastoSphere, mobile phase: methanol). To a solution of the residue obtained by concentration under reduced pressure in ethanol was added a solution of fumaric acid (33.7 mg) in ethanol. The mixture was concentrated under reduced pressure to give the title compound (130 mg).

Aufarbeitung

  1. customThe residue obtained by concentration under reduced pressure
  2. extractionwas desalted by a solid phase extraction resin (column
  3. extractionPL StrastoSphere solid phase extraction resin (PL-HCO3 MP StratoSpheres™), 500 mg
  4. customTo a solution of the residue obtained by concentration under reduced pressure in ethanol
  5. concentrationThe mixture was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-8aa8d611b2354113bb13f33cf758fbdb
Quelldatensatz
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08722662B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion