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

Ammonia → [4-(2-Azepan-1-ylethoxy)benzyl][5-methoxy-2-(6-methoxy-1,2,3,4-tetrahydronaphthalen-2-yl)phenyl]amine

HRID 2423722
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2423722
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl-].[Al+3].[Cl-].[Cl-].[N:11]1([CH2:18][CH2:19][O:20][C:21]2[CH:49]=[CH:48][C:24]([C:25]([NH:27][C:28]3[CH:33]=[C:32]([O:34][CH3:35])[CH:31]=[CH:30][C:29]=3[CH:36]3[CH2:45][CH2:44][C:43]4[C:38](=[CH:39][CH:40]=[C:41]([O:46][CH3:47])[CH:42]=4)[CH2:37]3)=O)=[CH:23][CH:22]=2)[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1.N>O1CCCC1>[N:11]1([CH2:18][CH2:19][O:20][C:21]2[CH:22]=[CH:23][C:24]([CH2:25][NH:27][C:28]3[CH:33]=[C:32]([O:34][CH3:35])[CH:31]=[CH:30][C:29]=3[CH:36]3[CH2:45][CH2:44][C:43]4[C:38](=[CH:39][CH:40]=[C:41]([O:46][CH3:47])[CH:42]=4)[CH2:37]3)=[CH:48][CH:49]=2)[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 222AmmoniaHCID 6451240Aluminum(III) ChlorideHCID 21226445Aluminium lithium hydrideHCID 666278204-(2-azepan-1-ylethoxy)-N-[5-methoxy-2-(6-methoxy-1,2,3,4-tetrahydronaphthalen-2-yl)phenyl]benzamide

Produkt 1

HCID 57933857[4-(2-Azepan-1-ylethoxy)benzyl][5-methoxy-2-(6-methoxy-1,2,3,4-tetrahydronaphthalen-2-yl)phenyl]amine
Ausbeute 77,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

To a suspension of 4-(2-azepan-1-ylethoxy)benzoic acid hydrochloride (300 mg) in 1,2-dichloroethane (15 ml) was added thionyl chloride (0.3 ml), the solution was refluxed for 40 minutes, then the reaction solution was concentrated in vacuo. To a suspension of the resulting 4-(2-azepan-1-ylethoxy)benzoyl chloride hydrochloride in 1,4-dioxane (4 ml) were added 5-methoxy-2-(6-methoxy-1,2,3,4-tetrahydronaphthalen-2-yl)phenylamine (150 mg) and N,N-diisopropylethylamine (1 ml), and the solution was stirred for 1.5 hours at 90° C. Water was added thereto followed by stirring, and the solution was extracted with ethyl acetate, then sequentially washed with water and brine, dried over anhydrous magnesium sulfate, and then the solvent was evaporated in vacuo. The residue was purified by NH silica gel column chromatography (hexane-ethyl acetate-methanol system) to provide 4-(2-azepan-1-ylethoxy)-N-[5-methoxy-2-(6-methoxy-1,2,3,4-tetrahydronaphthalen-2-yl)phenyl]benzamide (156 mg). To a suspension of lithium aluminum hydride (33 mg) in tetrahydrofuran (1.5 ml) was added aluminum chloride (116 mg) on an ice bath under a nitrogen atmosphere, the solution was stirred for 10 minutes at room temperature, 4-(2-azepan-1-ylethoxy)-N-[5-methoxy-2-(6-methoxy-1,2,3,4-tetrahydronaphthalen-2-yl)phenyl]benzamide (153 mg) was then added thereto, followed by stirring for 2 hours at room temperature. Tetrahydrofuran and aqueous ammonia were sequentially added thereto, the solution was filtered through celite pad, and then the solvent was evaporated in vacuo. The residue was purified by NH silica gel column chromatography (hexane-ethyl acetate-methanol system) to provide the title compound (116 mg).

Aufarbeitung

  1. stirringby stirring for 2 hours at room temperature
  2. filtrationthe solution was filtered through celite pad
  3. customthe solvent was evaporated in vacuo
  4. customThe residue was purified by NH silica gel column chromatography (hexane-ethyl acetate-methanol system)

Quellen und Nachweise

ORD-Eintrag
ord-eee3389e0554460da12f8391e67a9a06
Quelldatensatz
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07960412B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion