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

Ethanol → Unii-9tvu6uuo09

HRID 49528
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 49528
[C:1]([CH2:4][C:5]1[CH:6]=[CH:7][C:8]([O:25][CH3:26])=[C:9]([CH:24]=1)[C:10]([NH:12][CH2:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]([F:23])([F:22])[F:21])=[CH:16][CH:15]=1)=[O:11])(=[O:3])N.C([OH:29])C.[OH-].[Na+].O>C(OCC)C>[CH3:26][O:25][C:8]1[CH:7]=[CH:6][C:5]([CH2:4][C:1]([OH:29])=[O:3])=[CH:24][C:9]=1[C:10](=[O:11])[NH:12][CH2:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]([F:23])([F:22])[F:21])=[CH:16][CH:15]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 702EthanolHCID 962WaterHCID 14798Sodium HydroxideHCID 120946625-carbamoylmethyl-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide

Produkt 1

HCID 9799335Unii-9tvu6uuo09

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl Ether
Lösungsmittel

Versuchsvorschrift

To 700 mg of 5-carbamoylmethyl-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide were added 21 ml of ethanol, 7 ml of 1 mol/l aqueous solution of sodium hydroxide, and the mixture was refluxed for 18 hours. The reaction mixture was poured into water, washed with ethyl acetate, and further the aqueous layer was adjusted to pH value of 1 to 2 with 2 mol/l hydrochloric acid, which was then extracted with ethyl acetate. The organic layer was washed with water and saturated brine in sequence and dried again over anhydrous sodium sulfate. Solvent was distilled off under reduced pressure, and the residue obtained was suspended with diethyl ether to collect the crystals by filtration. The crystals obtained were recrystallized from methylene chloride to obtain 435 mg of aimed product as colorless crystals.

Aufarbeitung

  1. temperaturethe mixture was refluxed for 18 hours
  2. washwashed with ethyl acetate
  3. extractionwas then extracted with ethyl acetate
  4. washThe organic layer was washed with water and saturated brine in sequence
  5. dry with materialdried again over anhydrous sodium sulfate
  6. distillationSolvent was distilled off under reduced pressure
  7. customthe residue obtained
  8. customto collect the crystals
  9. filtrationby filtration
  10. customThe crystals obtained
  11. customwere recrystallized from methylene chloride

Quellen und Nachweise

ORD-Eintrag
ord-8bbdcd7f42744919a823864bb298ee42
Quelldatensatz
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06706763B1

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion