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

Ethyl chloroformate → N-(1-(4-((4-(4-fluorophenyl)piperazin-1-yl)methyl)phenyl)cyclopropyl)acetamide

HRID 1282111
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1282111
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][C:15]3[CH:20]=[CH:19][C:18]([C:21]4(C(O)=O)[CH2:23][CH2:22]4)=[CH:17][CH:16]=3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.C(Cl)(=O)[O:28][CH2:29][CH3:30].[N-:33]=[N+]=[N-].[Na+].C[Mg]I.[Cl-].[NH4+]>O.CC(C)=O.C1(C)C=CC=CC=1.C(N(CC)CC)C>[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:9][CH2:10][N:11]([CH2:14][C:15]3[CH:20]=[CH:19][C:18]([C:21]4([NH:33][C:29](=[O:28])[CH3:30])[CH2:22][CH2:23]4)=[CH:17][CH:16]=3)[CH2:12][CH2:13]2)=[CH:4][CH:3]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

10

Edukt 5

HCID 10928Ethyl chloroformateHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 184230631-(4-((4-(4-Fluorophenyl)piperazin-1-yl)methyl)phenyl)cyclopropanecarboxylic acidHCID 178418373HCID 178418373, Verbindung

Produkt 1

HCID 11523509
N-(1-(4-((4-(4-fluorophenyl)piperazin-1-yl)methyl)phenyl)cyclopropyl)acetamide

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 180AcetoneLösungsmittel3×HCID 962WaterLösungsmittel2×HCID 1140TolueneLösungsmittelHCID 8471TriethylamineLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a suspension of 1-(4-((4-(4-fluorophenyl)piperazin-1-yl)methyl)phenyl)cyclopropanecarboxylic acid (1.73 g) in water (1.7 ml) was added acetone (7 ml) and dissolved therein. A solution of triethylamine (0.75 ml) in acetone (10 ml) was added under ice-cooling and a solution of ethyl chlorocarbonate (0.56 ml) in acetone (4 ml) was added dropwise over 15 min. The mixture was stirred at 0° C. for 30 min. To this solution was added dropwise a solution of sodium azide (0.48 g) in water (3 ml) under ice-cooling over 10 min. The mixture was stirred for 30 min. The reaction mixture was poured into ice water (100 ml) and extracted with diethyl ether. The extract was dried over anhydrous magnesium sulfate and the solvent was evaporated to give an oil. The oil was dissolved in toluene (17 ml) and heated at 100° C. for 1 hr. The reaction mixture was ice-cooled and methylmagnesium iodide (1M, diethyl ether solution) (4.3 ml) was added. The mixture was stirred at room temperature for 30 min. The reaction mixture was poured into aqueous ammonium chloride and extracted with water and ethyl acetate (100 ml). The extract was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated and the obtained residue was purified by silica gel column chromatography (developing solvent; ethyl acetate:methanol=100:1) and recrystallized from ethyl acetate-isopropyl ether to give the title compound (0.52 g) as white crystals.

Aufarbeitung

  1. dissolutiondissolved
  2. temperaturecooling
  3. temperaturecooling over 10 min
  4. stirringThe mixture was stirred for 30 min
  5. extractionextracted with diethyl ether
  6. dry with materialThe extract was dried over anhydrous magnesium sulfate
  7. customthe solvent was evaporated
  8. customto give an oil
  9. temperatureheated at 100° C. for 1 hr
  10. temperaturecooled
  11. stirringThe mixture was stirred at room temperature for 30 min
  12. extractionextracted with water and ethyl acetate (100 ml)
  13. washThe extract was washed with saturated brine
  14. dry with materialdried over anhydrous magnesium sulfate
  15. customThe solvent was evaporated
  16. customthe obtained residue was purified by silica gel column chromatography (developing solvent; ethyl acetate:methanol=100:1)
  17. customrecrystallized from ethyl acetate-isopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-b949882a28764547b3e61d21bee38303
Quelldatensatz
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06455528B1

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion